Potassium Iodide → HCID 46832591、化合物

HRID 1667751ノート

反応式

HRID 1667751 の反応式
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]2[N:13]=[CH:12][N:11]([C:14]3[S:15][C:16]([C:26]([NH2:28])=[O:27])=[C:17]([C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=4)[N:18]=3)[C:10]=2[CH:29]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[OH:38][CH2:39][CH2:40][NH:41][CH2:42][CH2:43][OH:44]>CN(C)C=O>[OH:38][CH2:39][CH2:40][N:41]([CH2:42][CH2:43][OH:44])[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]2[N:13]=[CH:12][N:11]([C:14]3[S:15][C:16]([C:26]([NH2:28])=[O:27])=[C:17]([C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=4)[N:18]=3)[C:10]=2[CH:29]=1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 8113DiethanolamineHCID 11430Potassium CarbonateHCID 674272962-[6-(3-Chloro-propoxy)-benzoimidazol-1-yl]-4-(3-chloro-phenyl)-thiazole-5-carboxylic acid amide

生成物 1

HCID 46832591HCID 46832591、化合物収率 56.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 0.043 g (0.1 mmole) of 2-[6-(3-chloro-propoxy)-benzoimidazol-1-yl]-4-(3-chloro-phenyl)-thiazole-5-carboxylic acid amide (I.34a), 1 mL of dimethylformamide, 0.069 g (0.5 mmole) of potassium carbonate, 0.001 g of potassium iodide and 0.029 mL (0.3 mmole) of 2-(2-hydroxy-ethylamino)-ethanol was stirred at 100 degrees for 3 hours. The mixture was concentrated under reduced pressure, and diluted with 20 mL of water. The precipitate was collected by filtration and the solid triturated with diethyl ether to give 0.029 g of 2-(6-{3-[bis-(2-hydroxy-ethyl)-amino]-propoxy}-benzoimidazol-1-yl)-4-(3-chloro-phenyl)-thiazole-5-carboxylic acid amide (I.35) as a white powder. MH+/Z=516

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additiondiluted with 20 mL of water
  3. filtrationThe precipitate was collected by filtration
  4. customthe solid triturated with diethyl ether

出典と根拠

ORDレコード
ord-2063aee5b7894deb9ec8494200923fb0
出典データセット
uspto-grants-2011_10
特許番号
US08044213B2

反応ノート

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