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HCID 21834217,化合物 → HCID 57203651,化合物

HRID 1708994
笔记
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反应方程式

HRID 1708994 反应方程式
N[C:2]1[CH:3]=[CH:4][C:5]2[S:9][CH2:8][CH:7]([C:10]([N:12]([CH2:16][CH2:17][CH3:18])[CH2:13][CH2:14][CH3:15])=[O:11])[C:6]=2[CH:19]=1.N([O-])=[O:21].[Na+]>S(=O)(=O)(O)O.O>[OH:21][C:2]1[CH:3]=[CH:4][C:5]2[S:9][CH2:8][CH:7]([C:10]([N:12]([CH2:16][CH2:17][CH3:18])[CH2:13][CH2:14][CH3:15])=[O:11])[C:6]=2[CH:19]=1
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 2

HCID 21834217HCID 21834217,化合物HCID 23668193亚硝酸钠

产物 1

HCID 57203651HCID 57203651,化合物

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂3 次HCID 1118四氧化硫溶剂2 次

实验过程

11.6 g of 5-amino-2,3-dihydro-N,N-dipropyl-3-benzothiophencarboxamide were dissolved in a mixture of 4 ml of conc. sulphuric acid and 40 ml of water. 3.1 g of sodium nitrite dissolved in 10 ml of water were added dropwise below 10° C. with stirring. After addition the mixture was stirred for further 0.5 hours. The diazonium solution was then added carefully to a pre-heated solution of 50 ml of conc. sulphuric acid in 40 ml of water at 115°-120° C. The resulting mixture was poured onto ice and subsequently extracted with dichloromethane. Yield of the title compound as a semicrystalline product: 8.7 g.

后处理

  1. additionwere added dropwise below 10° C.
  2. additionAfter addition the mixture
  3. stirringwas stirred for further 0.5 hours
  4. additionThe resulting mixture was poured onto ice
  5. extractionsubsequently extracted with dichloromethane

来源与证据

ORD记录
ord-a4337253bd404ffd934c3c68591c4702
来源数据集
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
专利号
US04946863

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记