Triethylamine → HCID 86761807, 화합물

HRID 1968704노트

반응식

HRID 1968704 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][C:7]([CH2:11][OH:12])=[CH:8][CH:9]=2)[CH:4]=[N:3]1.C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22]>ClCCl>[CH3:20][S:21]([O:12][CH2:11][C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[N:2]([CH3:1])[N:3]=[CH:4]2)(=[O:23])=[O:22]

참가 물질

5

반응물 3

HCID 8471Triethylamine2회HCID 31297Methanesulfonyl chloride2회HCID 44119264(1-Methyl-1H-indazol-5-YL)methanol

생성물 1

HCID 86761807HCID 86761807, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

(1-methyl-1H-indazol-5-yl)methanol (0.15 g, 0.92 mmol) was dissolved in dichloromethane (3 mL), cooled to 0° C. and treated with triethylamine (0.14 mL, 1.0 mmol, 1.1 equiv) and methanesulfonyl chloride (0.079 mL, 1.0 mmol, 1.1 equiv). After stirring for 2 hours, the mixture was treated with additional triethylamine (0.14 mL, 1.0 mmol, 1.1 equiv) and methanesulfonyl chloride (0.079 mL, 1.0 mmol, 1.1 equiv). After an additional 1 hour, the mixture was diluted with dichloromethane (100 mL), washed with sodium bicarbonate (15 mL, aqueous saturated) and brine (15 mL), dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.

후처리

  1. waitAfter an additional 1 hour
  2. washwashed with sodium bicarbonate (15 mL, aqueous saturated) and brine (15 mL)
  3. dry with materialdried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-6ef102e6995b4214a0d5ae72b956290c
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08426438B2

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