HRID1974957

反应详情

EQUATION

反应方程式

HRID 1974957 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 3-t-butoxycarbonylaminothiophene-2-carboxylate (15.0 g, 58.3 mmol) was warmed in a mixture of 1 N sodium hydroxide (116.6 ml) and tetrahydrofuran (60 ml) at 50° C. for 16 hours. The mixture was evaporated to a volume of approximately 60 ml, and acidified (pH=2) with hydrochloric acid under cooling in an ice bath. The precipitate was filtered off, washed with water, and dried to afford 13.8 g (97%) of 3-t-butoxycarbonylaminothiophene-2-carboxylic acid. M.p. 168°-169° C. Litt. m.p. 168-169° C. (i. Chem. Res. (S) , 296, 1985). 1H-NMR (DMSO-D6, δ) : 1.49 (s, 9H), 7.76 (d, 1H), 7.85 (d, 1H), 9.45 (s, 1H), 13.45 (s, 1H) .

WORKUP

后处理

  1. customThe mixture was evaporated to a volume of approximately 60 ml
  2. temperatureunder cooling in an ice bath
  3. filtrationThe precipitate was filtered off
  4. washwashed with water
  5. customdried