Methyl 3-aminosulfonylthiophene-2-carboxylate → 2-(羟甲基)噻吩-3-磺酰胺

HRID 1252352

反应方程式

HRID 1252352 反应方程式
[NH2:1][S:2]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10](OC)=[O:11])(=[O:4])=[O:3].[BH4-].[Li+]>O1CCCC1>[OH:11][CH2:10][C:6]1[S:7][CH:8]=[CH:9][C:5]=1[S:2]([NH2:1])(=[O:4])=[O:3]

参与物

4

反应物 2

HCID 101012Methyl 3-aminosulfonylthiophene-2-carboxylateHCID 4148881硼氢化锂

产物 1

HCID 142549372-(羟甲基)噻吩-3-磺酰胺收率 41.2%

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂

实验过程

To 5.0 g of methyl 3-aminosulfonylthiophene-2-carboxylate in 200 mL of tetrahydrofuran was added 0.75 g of lithium borohydride. After heating at reflux for two hours the reaction was quenched with water and acidified with concentrated hydrochloric acid. The desired product was then extracted into methylene chloride which was washed with water, dried over magnesium sulfate, filtered and concentrated in vacuo to yield 1.8 g of a yellow solid, m.p. 85°-89°.

后处理

  1. temperatureAfter heating
  2. temperatureat reflux for two hours the reaction
  3. customwas quenched with water
  4. extractionThe desired product was then extracted into methylene chloride which
  5. washwas washed with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

来源与证据

ORD记录
ord-c05cdcf7574e4c4cb07a343f8ed48be9
来源数据集
uspto-grants-1988_05
专利号
US04743290

关联笔记

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