Triethylamine → methanesulfonic acid 1-methyl-1H-pyrazol-4-ylmethyl ester

HRID 246342

反応式

HRID 246342 の反応式
[CH3:1][N:2]1[CH:6]=[C:5]([CH2:7][OH:8])[CH:4]=[N:3]1.C(N(CC)CC)C.[CH3:16][S:17](Cl)(=[O:19])=[O:18]>C(Cl)Cl>[CH3:1][N:2]1[CH:6]=[C:5]([CH2:7][O:8][S:17]([CH3:16])(=[O:19])=[O:18])[CH:4]=[N:3]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 11961423(1-methyl-1H-pyrazol-4-yl)methanol

生成物 1

HCID 86677974methanesulfonic acid 1-methyl-1H-pyrazol-4-ylmethyl ester収率 86.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a partial suspension of (1-methyl-1H-pyrazol-4-yl)methanol (75 mg, 0.67 mmol) in CH2Cl2 (4 mL) at 0° C. was added triethylamine (0.19 mL, 1.34 mmol) followed by methanesulfonyl chloride (57 μL, 0.74 mmol). The cloudy reaction mixture was stirred at 0° C. for 1 h then quenched with water and extracted with CH2Cl2. The organics were dried over MgSO4 and concentrated to give 110 mg of methanesulfonic acid 1-methyl-1H-pyrazol-4-ylmethyl ester a colorless oil which was used without further purification.

後処理

  1. customThe cloudy reaction mixture
  2. customthen quenched with water
  3. extractionextracted with CH2Cl2
  4. dry with materialThe organics were dried over MgSO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-970c8880cb2a42609aec577bb9388b8c
出典データセット
uspto-grants-2014_02
特許番号
US08658646B2

関連ノート

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