Water → Methanesulfonic acid 1-pyrimidin-2-yl-piperidin-4-yl ester

HRID 1853372노트

반응식

HRID 1853372 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][CH:10]([OH:13])[CH2:9][CH2:8]1.C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23].O>ClCCl>[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:8][CH2:9][CH:10]([O:13][S:22]([CH3:21])(=[O:24])=[O:23])[CH2:11][CH2:12]1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 202340981-(Pyrimidin-2-yl)piperidin-4-ol

생성물 1

HCID 86673125Methanesulfonic acid 1-pyrimidin-2-yl-piperidin-4-yl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a cooled solution of 1-Pyrimidin-2-yl-piperidin-4-ol (WO2008/8895 A1), (100 mg; 0.55 mmol) and triethylamine (233 μL, 1.67 mmol) in dry dichloromethane (1 mL), was added methanesulfonyl chloride (52 μL, 0.67 mmol). The reaction mixture was stirred at room temperature for 5 hours. Water was added. After extraction with dichloromethane, the combined organic extracts were dried over sodium sulfate and concentrated to afford a crude product that was used in the next step without further purification.

후처리

  1. extractionAfter extraction with dichloromethane
  2. dry with materialthe combined organic extracts were dried over sodium sulfate
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-eaf8a611c1f04dc9a9b81630d20d065e
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962627B2

반응 노트

불러오는 중…