Triethylamine → Methanesulfonic acid (R)-3-(4-bromo-3,5-dimethyl-phenoxy)-2-methyl-propyl ester

HRID 237501ノート

反応式

HRID 237501 の反応式
[Br:1][C:2]1[C:13]([CH3:14])=[CH:12][C:5]([O:6][CH2:7][C@@H:8]([CH3:11])[CH2:9][OH:10])=[CH:4][C:3]=1[CH3:15].[CH3:16][S:17](Cl)(=[O:19])=[O:18].C(N(CC)CC)C>ClCCl>[Br:1][C:2]1[C:13]([CH3:14])=[CH:12][C:5]([O:6][CH2:7][C@@H:8]([CH3:11])[CH2:9][O:10][S:17]([CH3:16])(=[O:19])=[O:18])=[CH:4][C:3]=1[CH3:15]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 86697161(S)-3-(4-Bromo-3,5-dimethyl-phenoxy)-2-methyl-propan-1-ol

生成物 1

HCID 86697162Methanesulfonic acid (R)-3-(4-bromo-3,5-dimethyl-phenoxy)-2-methyl-propyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(S)-3-(4-Bromo-3,5-dimethyl-phenoxy)-2-methyl-propan-1-ol (130 mg), methanesulfonyl chloride (0.073 mL) and triethylamine (0.264 mL) are stirred in 5 mL of dichloromethane at room temperature overnight. The reaction mixture is washed with citric acid saturated aqueous solution and with brine. The organic phase is separated, dried over sodium sulfate and concentrated under vacuum to give the title compound, used in the next step without further purification. Yield: 148 mg.

後処理

  1. washThe reaction mixture is washed with citric acid saturated aqueous solution and with brine
  2. customThe organic phase is separated
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-aa5dc9ec9e18448b890e0546c1c88e69
出典データセット
uspto-grants-2014_02
特許番号
US08642585B2

反応ノート

読み込み中…