Methanesulfonyl chloride → 4-Benzoyl-1-methanesulphonylpiperidine

HRID 900757

반응식

HRID 900757 반응식
CCN(C(C)C)C(C)C.Cl.[C:11]1([C:17]([CH:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)=[O:18])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH3:25][S:26](Cl)(=[O:28])=[O:27]>C(Cl)Cl>[CH3:25][S:26]([N:22]1[CH2:23][CH2:24][CH:19]([C:17]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)=[O:18])[CH2:20][CH2:21]1)(=[O:28])=[O:27]

참가 물질

5

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 27244374-Benzoylpiperidine hydrochloride

생성물 1

HCID 160435364-Benzoyl-1-methanesulphonylpiperidine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Neat DIPEA (1.54 ml, 8.86 mmol) was added dropwise to a solution of phenyl(4-piperidinyl)methanone hydrochloride (1 g, 4.43 mmol) in CH2Cl2 (20 ml) at 0° C. Then, neat MsCl (377 μL, 4.87 mmol) was slowly added and the cooling bath was removed. After 30 minutes, the reaction was quenched with water and diluted with CH2Cl2. After separation, the organic phase was washed with brine, dried over MgSO4 and evaporated to dryness. The final ketone 1 was obtained as a white solid (1.16 g, 98%).

후처리

  1. customthe cooling bath was removed
  2. customthe reaction was quenched with water
  3. additiondiluted with CH2Cl2
  4. customAfter separation
  5. washthe organic phase was washed with brine
  6. dry with materialdried over MgSO4
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-aa78a692c2cb4f939b8c603d3c78b629
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07361668B2

연결된 노트

불러오는 중…