2-氨基-2-甲基-1-丙醇 → 4-tert-Butyl-N-(2-hydroxy-1,1-dimethyl-ethyl)-benzamide

HRID 68460

反应方程式

HRID 68460 反应方程式
[NH2:1][C:2]([CH3:6])([CH3:5])[CH2:3][OH:4].[C:7]([C:11]1[CH:19]=[CH:18][C:14]([C:15](Cl)=[O:16])=[CH:13][CH:12]=1)([CH3:10])([CH3:9])[CH3:8]>C(Cl)Cl>[C:7]([C:11]1[CH:12]=[CH:13][C:14]([C:15]([NH:1][C:2]([CH3:6])([CH3:5])[CH2:3][OH:4])=[O:16])=[CH:18][CH:19]=1)([CH3:10])([CH3:8])[CH3:9]

参与物

4

反应物 2

HCID 118072-氨基-2-甲基-1-丙醇HCID 74372对叔丁基苯甲酰氯

产物 1

HCID 3200764-tert-Butyl-N-(2-hydroxy-1,1-dimethyl-ethyl)-benzamide收率 105.5%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

30.95 g (347 mmol) of 2-amino-2-methyl-1-propanol was weighed into a 500 mL Erlenmeyer flask fitted with a stir bar and septum. Added 200 mL CH2Cl2. Established and maintained nitrogen atmosphere. Stirred the solution in an ice/water bath. Added 34 mL (174 mmol) of 4-tert-butylbenzoyl chloride dropwise over 30 min. A white precipitate formed. Stirred at room temperature overnight. Removed the solids by filtration and washed with CH2Cl2. Removed the solvent from the filtrate on rotavap and dried at 60°/4 torr to obtain 45.79 g of the title compound as a light yellow resin. MS (EST) 248 (M−H)−.

后处理

  1. customfitted with a stir bar
  2. temperatureEstablished and maintained nitrogen atmosphere
  3. customA white precipitate formed
  4. stirringStirred at room temperature overnight
  5. customRemoved the solids
  6. filtrationby filtration
  7. washwashed with CH2Cl2
  8. customRemoved the solvent from the filtrate on rotavap
  9. customdried at 60°/4 torr

来源与证据

ORD记录
ord-159bc30cce2642eea6900f4e4030b699
来源数据集
uspto-grants-2014_09
专利号
US08822457B2

关联笔记

加载中…