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

HRID 246342

반응식

HRID 246342 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-970c8880cb2a42609aec577bb9388b8c
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658646B2

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