Triethylamine → N-Cyclopropyl-N-(2-hydroxyethyl)-4-methoxy-2,6-dimethylphenylsulfonamide

HRID 45989ノート

反応式

HRID 45989 の反応式
[CH:1]1([NH:4][CH2:5][CH2:6][OH:7])[CH2:3][CH2:2]1.C(N(CC)CC)C.[CH3:15][O:16][C:17]1[CH:22]=[C:21]([CH3:23])[C:20]([S:24](Cl)(=[O:26])=[O:25])=[C:19]([CH3:28])[CH:18]=1>ClCCl>[CH:1]1([N:4]([CH2:5][CH2:6][OH:7])[S:24]([C:20]2[C:21]([CH3:23])=[CH:22][C:17]([O:16][CH3:15])=[CH:18][C:19]=2[CH3:28])(=[O:26])=[O:25])[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 159174964-Methoxy-2,6-dimethylbenzene-1-sulfonyl chlorideHCID 191005662-(Cyclopropylamino)ethan-1-ol

生成物 1

HCID 43577600N-Cyclopropyl-N-(2-hydroxyethyl)-4-methoxy-2,6-dimethylphenylsulfonamide収率 20%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
0 °C

実験手順

To a cold (0° C.) solution of 2-cyclopropylamino-ethanol (8 mmol) in dichloromethane (24 ml) and triethylamine (2.5 equiv.) a solution of 4-methoxy-2,6-dimethylbenzenesulfonyl chloride (7 mmol) in dichloromethane (12 ml) was added dropwise maintaining the temperature at 0° C. After complete addition the reaction mixture was stirred at 25° C. for 90 min by which time the reaction was complete (TLC). The reaction mixture was diluted with dichloromethane (200 ml) and washed with water and finally with brine. The organic layer was dried over sodium sulfate and evaporated to dryness to obtain the pure product. Yield: 20%

後処理

  1. additionAfter complete addition the reaction mixture
  2. washwashed with water and finally with brine
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. customevaporated to dryness
  5. customto obtain the pure product

出典と根拠

ORDレコード
ord-31017654e9994e0384e8f0702a1bee12
出典データセット
uspto-grants-2013_09
特許番号
US08541573B2

反応ノート

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