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Sodium Methoxide → HCID 178447401、化合物

HRID 1707445
ノート
印刷プレビュー

反応式

HRID 1707445 の反応式
C([S:4][CH2:5][S:6][C:7]1[N:8]=[N:9][NH:10][CH:11]=1)(=O)C.C[O-].[Na+].[C:15]1([CH:21]([O:28][C:29]([C:31]2[N:36]3[C:37](=[O:59])[C@@H:38]([NH:39][C:40](=[O:58])/[C:41](/[C:45]4[N:46]=[C:47]([NH:50][C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])[S:48][CH:49]=4)=[CH:42]\[CH2:43][CH3:44])[C@H:35]3[S:34][CH2:33][C:32]=2OS(C)(=O)=O)=[O:30])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>CN(C)C=O.CO.Cl.O>[C:15]1([CH:21]([O:28][C:29]([C:31]2[N:36]3[C:37](=[O:59])[C@@H:38]([NH:39][C:40](=[O:58])/[C:41](/[C:45]4[N:46]=[C:47]([NH:50][C:51]([O:53][C:54]([CH3:56])([CH3:57])[CH3:55])=[O:52])[S:48][CH:49]=4)=[CH:42]\[CH2:43][CH3:44])[C@H:35]3[S:34][CH2:33][C:32]=2[S:4][CH2:5][S:6][C:7]2[N:8]=[N:9][NH:10][CH:11]=2)=[O:30])[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 10942334Sodium MethoxideHCID 883012357beta-[(Z)-2-(2-t-butoxycarbonylaminothiazol-4-yl)-2-pentenoylamino]-3-methanesulfonyloxy-3-cephem-4-carboxylic acid diphenylmethyl esterHCID 178477162HCID 178477162、化合物

生成物 1

HCID 178447401HCID 178447401、化合物収率 70%

試薬・触媒・溶媒 4

HCID 313
Hydrochloric Acid
溶媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 4-acetylthiomethylthio-1,2,3-triazole (230 mg: 1.22 mMol.) in dimethylformamide (6 ml) is dropwise added a 1.26N-sodium methoxide in methanol (1.9 ml) at -60° C., and the mixture is stirred for 20 minutes, mixed with a solution of 7β-[(Z)-2-(2-t-butoxycarbonylaminothiazol-4-yl)-2-pentenoylamino]-3-methanesulfonyloxy-3-cephem-4-carboxylic acid diphenylmethyl ester (740 mg: 1 mMol.) in dimethylformamide (3 ml), and stirred at the same temperature for 40 minutes. The reaction mixture is diluted with 10% hydrochloric acid (2 ml) and water (30 ml) and extracted with ethyl acetate. The extract is washed with water, dried over sodium sulfate, and purified by silica gel chromatography (toluene: ethyl acetate=2:1) to give 7β-[(Z)-2-(2-t-butoxycarbonylaminothiazol-4-yl)-2-pentenoylamino]-3-(1,2,3-triazol-4-ylthiomethylthio)-3-cephem-4-carboxylic acid diphenylmethyl ester (553 mg) as colorless foam. Yield: 70%.

後処理

  1. stirringstirred at the same temperature for 40 minutes
  2. extractionextracted with ethyl acetate
  3. washThe extract is washed with water
  4. dry with materialdried over sodium sulfate
  5. custompurified by silica gel chromatography (toluene: ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-82de7460da3747eeb52fe2bb53caecbd
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05352792

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート