成盐反应

Query

Query Results Date

1. Query 19 reactions in

2014-11-18 01h:54m:50s (EST)

Reaxys

Search as: Product, As drawn, No salts, No mixtures

色氨酸甲酯盐酸盐的制备

在冰浴下,增加了100毫升圆底烧瓶与60毫升的甲醇,然后慢慢加4毫升SOCl2 恒压滴液漏斗(干燥管顶部),和氢氧化钠溶液吸收废气。

搅拌1小时后,8mmol的色氨酸(3 d)补充道,在室温下搅拌30分钟,然后回流在66°c 6 h。

反应是由薄层色谱跟踪,直到原料消失,2%茚三酮在乙醇溶液为显色剂。

溶剂蒸发了获得色氨酸甲酯盐酸盐。收益率:100%。

+→

Rx-ID: 3829969 View in Reaxys 1/19 Yield Conditions & References

100 % thionyl chloride, Time= 4h, Heating

; Tetrahedron; 57; nb. 51; (2001); p. 10181 - 10189View in Reaxys

100 %

(2) Preparation of L-Tryptophan Methyl Ester Hydrochloride Under ice bath, 100 ml round-bottom flask was added

with 60 ml of methanol, and then slowly added with 4 ml of SOClthrough constant pressure dropping funnel (with a

drying tube on the top), and NaOH solution was used to absorb exhaust. After stirring for 1 h, 8 mmol of L-

tryptophan (3d) was added and stirred at room temperature for 30 min, and then refluxed at 66° C. for 6 h. The

reaction was tracked by TLC until the raw material disappears, with a solution of 2percent ninhydrin in ethanol as

chromogenic reagent. The solvent was evaporated out to obtain L-tryptophan methyl ester hydrochloride. Yield:

100percent.

thionyl chloride methanol, ethanol, Time= 1h, Cooling with ice, Time= 6.5h, T= 20 - 66 °C

; ; US2014/206741; (2014); (A1) English View in Reaxys

98 % thionyl chloride, Time= 8h, Heating

; Organic Preparations and Procedures International; 33; nb. 4; (2001); p. 341 - 349View in Reaxys

98 % thionyl chloride, T= 0 - 60 °C

; ACS Medicinal Chemistry Letters; 4; nb. 2; (2013); p. 235 - 238View in Reaxys

97 % thionyl chloride, Time= 24h, T= -15 - 20 °C , Saturated gas, Inert atmosphere

; Chemical Communications; 50; nb. 23; (2014); p. 3052 - 3054View in Reaxys

96 % thionyl chloride, Time= 0.666667h, T= 25 - 30 °C , microwave irradiation

; Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry; 45; nb. 8; (2006); p. 1942 - 1944View

in Reaxys

95 % acetyl chloride

; Journal of Medicinal Chemistry; 57; nb. 8; (2014); p. 3324 - 3341View in Reaxys

93 % thionyl chloride, T= 5 °C , RefluxTime= 4h, Reflux

; Chirality; 25; nb. 10; (2013); p. 656 - 662View in Reaxys

92 % thionyl chloride, Time= 6.5h, T= -10 - 25 °C

; Journal of Chemical Information and Modeling; 53; nb. 1; (2013); p. 176 - 187View in Reaxys

73 % thionyl chloride, Time= 7h, T= 60 - 70 °C

; Bioorganic and Medicinal Chemistry; 15; nb. 14; (2007); p. 4903 - 4909View in Reaxys

67 % thionyl chloride, Time= 9h, T= 20 °C

; Dalton Transactions; 40; nb. 18; (2011); p. 5018 - 5025View in Reaxys

63 % hydrogenchloride, T= 0 °C

; Archiv der Pharmazie; 344; nb. 8; (2011); p. 494 - 504View in Reaxys