Water → HCID 53417180, 화합물

HRID 1844701

반응식

HRID 1844701 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([Br:11])[CH:10]=1)[C:5](O)=[O:6].Cl.[CH3:13][NH:14][O:15][CH3:16].C(N=[N+]=[N-])C.O>O=S(Cl)Cl.C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([Br:11])[CH:10]=1)[C:5]([N:14]([O:15][CH3:16])[CH3:13])=[O:6]

참가 물질

7

반응물 4

HCID 962WaterHCID 12063Benzoic acid, 3,5-dibromo-HCID 79118Ethane, azido-HCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)

생성물 1

HCID 53417180HCID 53417180, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 24386Thionyl Chloride용매

실험 절차

The solution of 3,5-dibromobenzoic acid (26 g, 93 mmol) in SOCl2 (100 mL) was heated at reflux for 2 h, concentrated, diluted with dry DCM (300 mL) and added slowly to a stirred solution of N,O-dimethylhydroxylamine hydrochloride (9.75 g, 100 mmol) and EtN3 (28 g, 277 mmol) in dry DCM (300 mL) at 0° C. The solution was stirred for 1 h at rt, poured into water and the organic layer was separated. The organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated to give crude compound P37a (28 g, 93%) as an oil.

후처리

  1. temperatureat reflux for 2 h
  2. concentrationconcentrated
  3. additiondiluted with dry DCM (300 mL)
  4. customthe organic layer was separated
  5. washThe organic layer was washed with water and brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give crude compound P37a (28 g, 93%) as an oil

출처 및 근거

ORD 기록
ord-a71840bae54548e9944a5090f50bb903
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946446B2

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