Triethylamine → HCID 57885697, 화합물
반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][OH:9])[CH:5]=[N:6][CH:7]=1.C(N(CC)CC)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][O:9][S:18]([CH3:17])(=[O:20])=[O:19])[CH:5]=[N:6][CH:7]=1참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
To the stirred solution (5-bromo-pyridin-3-yl)-methanol (3.0 g, 16 mmol) in CH2Cl2 (30 mL) is added triethylamine (2.4 g, 24 mmol). The reaction mixture is cooled to 0° C., methanesulfonyl chloride (2.2 g, 19 mmol) is added slowly at 0° C. Then the reaction mixture is warmed up to room temperature for 3 hrs. Ice cold water is added and the mixture is extracted with CH2Cl2. Organic layers are combined, dried over Na2SO4 and concentrated to give 3.0 g of the crude methanesulfonic acid 5-bromo-pyridin-3-ylmethyl ester which is used without purification.
후처리
- temperatureThen the reaction mixture is warmed up to room temperature for 3 hrs
- additionIce cold water is added
- extractionthe mixture is extracted with CH2Cl2
- dry with materialdried over Na2SO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-4cd3dc14a3a54987893e1c3a9e8e9e07
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09181272B2
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