5-Bromo-6-chloropyridine-3-sulfonyl chloride → 5-(Azetidine-1-sulfonyl)-3-bromo-2-chloropyridine

HRID 1989904노트

반응식

HRID 1989904 반응식
Cl.[NH:2]1[CH2:5][CH2:4][CH2:3]1.[Br:6][C:7]1[C:8]([Cl:17])=[N:9][CH:10]=[C:11]([S:13](Cl)(=[O:15])=[O:14])[CH:12]=1>C(Cl)Cl.N1C=CC=CC=1>[N:2]1([S:13]([C:11]2[CH:12]=[C:7]([Br:6])[C:8]([Cl:17])=[N:9][CH:10]=2)(=[O:15])=[O:14])[CH2:5][CH2:4][CH2:3]1

참가 물질

5

반응물 2

HCID 27936265-Bromo-6-chloropyridine-3-sulfonyl chlorideHCID 12308726Azetidine hydrochloride

생성물 1

HCID 536296285-(Azetidine-1-sulfonyl)-3-bromo-2-chloropyridine수율 37.3%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매

실험 절차

Azetidine hydrochloride (0.32 g, 3.44 mmol) was added to a solution of 3-bromo-2-chloropyridine-5-sulfonyl chloride (1 g, 3.44 mmol) in DCM (4 mL) and pyridine (10 mL) and stirred at RT for 22 hours. The solvent was removed in vacuo and ethyl acetate (30 mL) added. The organic phase was washed with 1M hydrochloric acid (20 mL), water (20 mL), brine (20 mL), dried (MgSO4), filtered and the solvent removed in vacuo to give the desired compound (0.4 g).

후처리

  1. customThe solvent was removed in vacuo and ethyl acetate (30 mL)
  2. additionadded
  3. washThe organic phase was washed with 1M hydrochloric acid (20 mL), water (20 mL), brine (20 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-1aeb25c97e474e509802cdef48aa668b
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642263B2

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