叔丁醇 → N,N-diethyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4-amine

HRID 22787

反应方程式

HRID 22787 反应方程式
Cl[C:2]1[C:3]2[C:10]3[CH2:11][CH2:12][CH2:13][C:9]=3[S:8][C:4]=2[N:5]=[CH:6][N:7]=1.[CH2:14]([NH:16][CH2:17][CH3:18])[CH3:15].[C:19](O)(C)(C)C.CCOC(C)=O>O.Cl>[CH2:14]([N:16]([CH2:17][CH3:18])[C:2]1[C:3]2[C:10]3[CH2:19][CH2:11][CH2:12][CH2:13][C:9]=3[S:8][C:4]=2[N:5]=[CH:6][N:7]=1)[CH3:15]

参与物

6

反应物 4

HCID 6386叔丁醇HCID 8021二乙胺2 次HCID 8857乙酸乙酯HCID 7898174-氯-6,7-二氢-5H-环戊并[4,5]噻吩并[2,3-D]嘧啶

产物 1

HCID 717848N,N-diethyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4-amine

试剂、催化剂与溶剂 1

HCID 21885828Hydrate;hydrochloride溶剂

实验过程

To a slurry of 0.044 g 4-chloro-6,7-dihydro-5H-cyclopenta[4,5]thieno[2,3-d]pyrimidine (0.196 mmol) in 1 mL of 100:1 H2O/HCl was added 0.014 g (0.02 mL, 0.106 mmol) diethylamine. The mixture was heated to reflux, and an additional 0.2 mL diethylamine and 1 mL of t-butanol were added and heated continued at reflux for an additional 1 h. TLC (20% EtOAc/80% pet ether) showed complete reaction and the 1H NMR of the isolated material was consistent with the desired product.

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureheated
  4. temperatureat reflux for an additional 1 h
  5. customreaction

来源与证据

ORD记录
ord-dcfb3b429c2544d6bb6f40646bccd630
来源数据集
uspto-grants-2005_02
专利号
US06849638B2

关联笔记

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