Water → HCID 54430516、化合物

HRID 233491ノート

反応式

HRID 233491 の反応式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[OH:12][CH2:13][CH2:14][NH:15][CH2:16][C:17]([CH3:20])([OH:19])[CH3:18].[OH2:21]>N1C=CC=CC=1>[CH3:11][C:1]1[CH:6]=[CH:5][C:4]([S:7]([N:15]([CH2:16][C:17]([CH3:20])([OH:19])[CH3:18])[CH2:14][CH2:13][O:12][S:7]([C:4]2[CH:5]=[CH:6][C:1]([CH3:11])=[CH:2][CH:3]=2)(=[O:8])=[O:21])(=[O:9])=[O:8])=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 149870161-[(2-Hydroxyethyl)amino]-2-methyl-2-propanol

生成物 1

HCID 54430516HCID 54430516、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

4-Toluenesulfonyl chloride (166.1 g) was added portionwise to a stirred solution of 1-[(2-hydroxyethyl)amino]-2-methyl-2-propanol (58.0 g) in pyridine (275 ml) at 0°-10° C. The resulting solution was stirred at room temperature for 15 h and then poured into water (1 l). The mixture was extracted with dichloromethane and the organic phase was washed with hydrochloric acid (2.5M) and brine. After drying over magnesium sulfate, the solvent was removed under reduced pressure to give 1-{N-[(4-methylphenyl)sulfonyl]-N-[(4-methylphenyl)sulfonyloxyethyl]amino}-2-methyl-2-propanol (155.8 g). δ (CDCl3) 1.23 (s,6H), 2.44,2.46 (6H), 3.08 (s,2H), 3.45 (t,2H), 4.35 (t,2H) and 7.25-7.85 (m,8H).

後処理

  1. extractionThe mixture was extracted with dichloromethane
  2. washthe organic phase was washed with hydrochloric acid (2.5M) and brine
  3. dry with materialAfter drying over magnesium sulfate
  4. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-0ef93d24f82a486092953910db92c95c
出典データセット
uspto-grants-1997_01
特許番号
US05593983

反応ノート

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