Potassium Carbonate → HCID 10139190、化合物

HRID 1181325ノート

反応式

HRID 1181325 の反応式
C([O:4][C:5]1[CH:6]=[C:7]([O:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[N:22]([CH:23]4[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]4)[C:21]4[CH:29]=[CH:30][C:31]([C:33]([O:35][CH2:36][CH3:37])=[O:34])=[CH:32][C:20]=4[N:19]=3)=[CH:14][CH:13]=2)[CH:8]=[CH:9][CH:10]=1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO.O1CCCC1>[CH:23]1([N:22]2[C:21]3[CH:29]=[CH:30][C:31]([C:33]([O:35][CH2:36][CH3:37])=[O:34])=[CH:32][C:20]=3[N:19]=[C:18]2[C:15]2[CH:14]=[CH:13][C:12]([O:11][C:7]3[CH:8]=[CH:9][CH:10]=[C:5]([OH:4])[CH:6]=3)=[CH:17][CH:16]=2)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]1

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 10228675HCID 10228675、化合物

生成物 1

HCID 10139190HCID 10139190、化合物収率 97.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl 2-[4-(3-acetoxyphenyloxy)phenyl]-1-cyclohexylbenzimidazole-5-carboxylate (87 g) obtained in Example 27 was dissolved in methyl alcohol (250 ml) and tetrahydrofuran (250 ml), and potassium carbonate (31 g) was added. The mixture was stirred for 30 min at room temperature. The insoluble materials were filtered off and the filtrate was concentrated under reduced pressure. Water was added to the residue and the mixture was neutralized with 2N hydrochloric acid. The precipitated crystals were collected by filtration to give the title compound (78 g, yield 97%).

後処理

  1. filtrationThe insoluble materials were filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionWater was added to the residue
  4. filtrationThe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-0e06dde6754e496c88b8bb3249bd7b5b
出典データセット
uspto-grants-2007_10
特許番号
US07285551B2

反応ノート

読み込み中…