氨 → tert-Butyl (5-bromo-2-carbamoylthiophen-3-yl)carbamate

HRID 11424

反应方程式

HRID 11424 反应方程式
[Br:1][C:2]1[S:6][C:5]([C:7](O)=[O:8])=[C:4]([NH:10][C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH:3]=1.OC1C2N=N[NH:24]C=2C=CC=1.Cl.CN(C)CCCN=C=NCC.N>C(#N)C>[Br:1][C:2]1[S:6][C:5]([C:7]([NH2:24])=[O:8])=[C:4]([NH:10][C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH:3]=1

参与物

6

反应物 4

HCID 222氨HCID 27239391-乙基-(3-二甲基氨基丙基)碳酰二亚胺盐酸盐HCID 219758545-溴-3-((叔丁氧基羰基)氨基)噻吩-2-羧酸HCID 178418300HCID 178418300，化合物

产物 1

HCID 21975856tert-Butyl (5-bromo-2-carbamoylthiophen-3-yl)carbamate

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

5-Bromo-3-[(t-butyloxycarbonyl)amino]thiophene-2-carboxylic acid (0.80 g) was stirred in acetonitrile (80 ml). Hydroxybenztriazole (1.41 g) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.62 g) were added and stirring continued at room temperature for 10 minutes. Concentrated aqueous ammonia solution (8 ml) was added and the reaction mixture was heated to reflux for 1 h. The acetonitrile was removed by evaporation. Water (100 ml) was added and the mixture was sonicated and triturated. The resultant off-white solid was then collected by filtration, washed with water and dried under vacuum (0.763 g).

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 1 h
  3. customThe acetonitrile was removed by evaporation
  4. additionWater (100 ml) was added
  5. customthe mixture was sonicated
  6. customtriturated
  7. filtrationThe resultant off-white solid was then collected by filtration
  8. washwashed with water
  9. customdried under vacuum (0.763 g)

来源与证据

ORD记录
ord-0290ac04ad0e445e81e62a6c3df508c9
来源数据集
uspto-grants-2006_08
专利号
US07098240B2

关联笔记

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