甲苯 → Ethyl 2-[6-fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-ylaminothiocarbonyl]hexahydropyridazine-1-carboxylate

HRID 1761810笔记

反应方程式

HRID 1761810 反应方程式
[F:1][C:2]1[C:14]([N:15]=[C:16]=[S:17])=[CH:13][C:5]2[N:6]([CH2:10][CH:11]=[CH2:12])[C:7](=[O:9])[S:8][C:4]=2[CH:3]=1.[N:18]1([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:23][CH2:22][CH2:21][CH2:20][NH:19]1.C1(C)C=CC=CC=1.C(N(CC)CC)C>O>[F:1][C:2]1[C:14]([NH:15][C:16]([N:19]2[CH2:20][CH2:21][CH2:22][CH2:23][N:18]2[C:24]([O:26][CH2:27][CH3:28])=[O:25])=[S:17])=[CH:13][C:5]2[N:6]([CH2:10][CH:11]=[CH2:12])[C:7](=[O:9])[S:8][C:4]=2[CH:3]=1

参与物

6

反应物 4

HCID 1140甲苯HCID 8471三乙胺HCID 30143771(2H)-Pyridazinecarboxylic acid, tetrahydro-, ethyl esterHCID 143064856-Fluoro-3-(2propenyl)-2(3H)-benzothiazolon-5-yl isothiocyanate

产物 1

HCID 14306486Ethyl 2-[6-fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-ylaminothiocarbonyl]hexahydropyridazine-1-carboxylate收率 105.1%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

6-Fluoro-3-(2propenyl)-2(3H)-benzothiazolon-5-yl isothiocyanate (3.1 g) and ethyl hexahydropyridazine-1-carboxylate (1.17 g) were added to toluene (15 ml). A catalytic amount of triethylamine was added thereto, and the resultant mixture was stirred at 25° C. for 12 hours. Water was added thereto, and the resultant mixture was extracted with toluene. The extract was washed with water, dried and concentrated to give ethyl 2-[6-fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-ylaminothiocarbonyl]-hexahydropyridazine-1-carboxylate (3.3 g). m.p., 40°-42° C.

后处理

  1. extractionthe resultant mixture was extracted with toluene
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated

来源与证据

ORD记录
ord-d67269f353a64a339754b05b3cabc93c
来源数据集
uspto-grants-1989_05
专利号
US04828605

反应笔记

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