Water → HCID 53417180、化合物

HRID 1844701

反応式

HRID 1844701 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 53417180HCID 53417180、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 24386Thionyl Chloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a71840bae54548e9944a5090f50bb903
出典データセット
uspto-grants-2015_02
特許番号
US08946446B2

関連ノート

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