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Pyridine → HCID 54142886、化合物

HRID 1108490
ノート
印刷プレビュー

反応式

HRID 1108490 の反応式
[OH:1][CH:2]([C:15]1[C:24]([CH3:25])=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][C:16]=1[CH3:26])[C:3]1[CH:8]=[C:7]([N:9]2[CH:13]=[CH:12][N:11]=[CH:10]2)[CH:6]=[CH:5][C:4]=1[CH3:14].N1C=CC=CC=1.[CH3:33][C:34]1[CH:39]=[CH:38][C:37]([S:40]([NH:43][C@@H:44]([CH3:48])[C:45](Cl)=[O:46])(=[O:42])=[O:41])=[CH:36][CH:35]=1>ClC(Cl)C>[N:9]1([C:7]2[CH:6]=[CH:5][C:4]([CH3:14])=[C:3]([CH:8]=2)[CH:2]([C:15]2[C:16]([CH3:26])=[CH:17][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:23][C:24]=2[CH3:25])[O:1][C:45](=[O:46])[C@@H:44]([NH:43][S:40]([C:37]2[CH:38]=[CH:39][C:34]([CH3:33])=[CH:35][CH:36]=2)(=[O:42])=[O:41])[CH3:48])[CH:13]=[CH:12][N:11]=[CH:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 10882640Methyl (+/-)-4-[alpha-hydroxy-5-(1-imidazolyl)-2-methylbenzyl]-3,5-dimethylbenzoateHCID 12924680HCID 12924680、化合物

生成物 1

HCID 54142886HCID 54142886、化合物収率 100.9%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒2 回

実験手順

Methyl (±)-4-[α-hydroxy-5-(1-imidazolyl)-2-methylbenzyl]-3,5-dimethylbenzoate (35 g) was suspended in dichloroethane (350 ml) and pyridine (12 ml) and a solution of (S)-2-(4-methylbenzenesulfonylamino)propionyl chloride (31.4 g) in dichloroethane (70 ml) was added dropwise to the suspension over 10 minutes with stirring under ice-cooling. The mixture was stirred at room temperature for 4 hours, and the reaction mixture was washed successively with water, 5% citric acid, 5% potassium carbonate and water. The organic layer was separated and dried over magnesium sulfate. The solvent was evaporated under reduced pressure to give 58 g of methyl (±)-4-[5-(1-imidazolyl)-2-methyl-α-{(S)-2-(4-methylbenzenesulfonylamino)propionyloxy}benzyl]-3,5-dimethylbenzoate as a pale-yellow oil. This was crystallized from ethyl acetate (120 ml) and isopropyl ether (480 ml), and the obtained crystals were recrystallized from ethyl acetate (50 ml) and isopropyl ether (100 ml) to give 20 g of methyl (S)-4-[5-(1-imidazolyl)-2-methyl-α-{(S)-2-(4-methylbenzenesulfonylamino)propionyloxy}benzyl]-3,5-dimethylbenzoate as white crystals, melting point 103-105° C.

後処理

  1. temperaturecooling
  2. stirringThe mixture was stirred at room temperature for 4 hours
  3. washthe reaction mixture was washed successively with water, 5% citric acid, 5% potassium carbonate and water
  4. customThe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-1d1c4b115cd04cae9d58a158ac4d1221
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06066739

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