4-Toluenesulfonyl chloride → HCID 86659055、化合物

HRID 2407678ノート

反応式

HRID 2407678 の反応式
C(N(CC)CC)C.[C:8]1([CH3:18])[CH:13]=[CH:12][C:11]([S:14](Cl)(=[O:16])=[O:15])=[CH:10][CH:9]=1.[C:19]1([C:25]2[CH:29]=[C:28]([CH2:30][N:31]3[CH2:36][CH2:35][CH:34]([CH2:37][OH:38])[CH2:33][CH2:32]3)[O:27][N:26]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>ClCCl>[CH3:18][C:8]1[CH:13]=[CH:12][C:11]([S:14]([O:38][CH2:37][CH:34]2[CH2:33][CH2:32][N:31]([CH2:30][C:28]3[O:27][N:26]=[C:25]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:29]=3)[CH2:36][CH2:35]2)(=[O:16])=[O:15])=[CH:10][CH:9]=1

参加物

5

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 52234807HCID 52234807、化合物

生成物 1

HCID 86659055HCID 86659055、化合物収率 12.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Triethylamine (12.1 mL) and p-toluene sulfonylchloride (6.61 g) were added sequentially to a room temperature mixture of the compound prepared in Example 64 (7.86 g) in dichloromethane (100 mL). The reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with dichloromethane and washed sequentially with a saturated aqueous sodium bicarbonate solution and brine. The combined organics were dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel to obtain the title compound (1.52 g) having the following physical data.

後処理

  1. washwashed sequentially with a saturated aqueous sodium bicarbonate solution and brine
  2. dry with materialThe combined organics were dried over anhydrous magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-96c5c674ca754ab3beeab4481d0c4685
出典データセット
uspto-grants-2014_08
特許番号
US08809538B2

反応ノート

読み込み中…