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

HRID 1989904ノート

反応式

HRID 1989904 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1aeb25c97e474e509802cdef48aa668b
出典データセット
uspto-grants-2010_01
特許番号
US07642263B2

反応ノート

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