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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 2-Chloro-N-[(2,2-difluoro-benzo[1,3]dioxol-5-ylamino)-methylsulfanyl-methyl]-6-methyl-isonicotinamide

HRID 1952182
笔记
打印预览

反应方程式

HRID 1952182 反应方程式
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[C:8]([C:10]([NH:12][C:13]([NH:15][C:16]2[CH:26]=[CH:25][C:19]3[O:20][C:21]([F:24])([F:23])[O:22][C:18]=3[CH:17]=2)=[S:14])=[O:11])[CH:7]=[C:6]([CH3:27])[N:5]=1.[CH3:28]I.O>C1COCC1>[Cl:3][C:4]1[CH:9]=[C:8]([CH:7]=[C:6]([CH3:27])[N:5]=1)[C:10]([NH:12][CH:13]([NH:15][C:16]1[CH:26]=[CH:25][C:19]2[O:20][C:21]([F:24])([F:23])[O:22][C:18]=2[CH:17]=1)[S:14][CH3:28])=[O:11]
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

6

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 6328碘甲烷HCID 24758氢化钠HCID 594977661-(2-Chloro-6-methyl-pyridine-4-carbonyl)-3-(2,2-difluoro-benzo[1,3]dioxol-5-yl)thiourea

产物 1

HCID 866457122-Chloro-N-[(2,2-difluoro-benzo[1,3]dioxol-5-ylamino)-methylsulfanyl-methyl]-6-methyl-isonicotinamide

试剂、催化剂与溶剂 1

HCID 8028
四氢呋喃
溶剂

反应条件

温度
0 °C

实验过程

NaH, 60% (2.2 g; 0.0550 mol) was stirred in THF (170 ml) on an ice bath under N2. Intermediate D1 (19.3 g; 0.500 mol) was then added and stirred for 1 hour at 0° C. CH3I (7.8 g; 0.0550 mol) was then added and the reaction mixture was allowed to warm to room temperature overnight. Water was added and the THF was evaporated in vacuo. The precipitate was filtered off, washed with water and dried. Yield: 22.86 g of intermediate D2.

后处理

  1. temperatureto warm to room temperature overnight
  2. customthe THF was evaporated in vacuo
  3. filtrationThe precipitate was filtered off
  4. washwashed with water
  5. customdried

来源与证据

ORD记录
ord-b819fa53071144cf83e50504fc5ea6e1
来源数据集
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08404851B2

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记