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Sodium hydride → HCID 68642095、化合物

HRID 1498948
ノート
印刷プレビュー

反応式

HRID 1498948 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[S:10][C:11]([C:15]([O:20][CH3:21])([O:18][CH3:19])[CH2:16][OH:17])=[C:12]([CH3:14])[N:13]=1.[CH3:22][O:23][C:24]1[CH:31]=[CH:30][C:27]([CH2:28]Cl)=[CH:26][CH:25]=1.[H-].[Na+]>CN(C)C=O>[CH3:21][O:20][C:15]([C:11]1[S:10][C:9]([C:3]2[CH:4]=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=2[CH3:1])=[N:13][C:12]=1[CH3:14])([O:18][CH3:19])[CH2:16][O:17][CH2:28][C:27]1[CH:30]=[CH:31][C:24]([O:23][CH3:22])=[CH:25][CH:26]=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 24758Sodium hydrideHCID 699934-Methyloxybenzyl chlorideHCID 68642113HCID 68642113、化合物

生成物 1

HCID 68642095HCID 68642095、化合物収率 64.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To N,N-dimethylformamide (2 ml), 2-[2-(2,4-dimethylphenyl)-4-methylthiazol-5-yl]-2,2-dimethoxyethanol (100 mg) prepared in the Step 31-1-2 and 4-methoxybenzyl chloride (61 mg) were added, and 60% sodium hydride suspension in oil (20 mg) was added thereto under an argon atmosphere. Then, the mixture was stirred at a room temperature for 4 hours. Ice water was added to the reaction solution, and then the mixture was subjected to extraction with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and then concentrated under a reduced pressure. The residue was purified by thin-layer chromatography (hexane:ethyl acetate=3:1) to give the title compound (90 mg, 64%).

後処理

  1. additionwere added
  2. extractionthe mixture was subjected to extraction with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under a reduced pressure
  5. customThe residue was purified by thin-layer chromatography (hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-67eab2ab8c65418092181b1f499b25c7
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09200008B2

反応ノート

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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