Hydrazine hydrate (1:1) → HCID 178434515、化合物

HRID 45514

反応式

HRID 45514 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=O)[CH3:10])=[CH:4][CH:3]=1.COC(OC)[N:15]([CH3:17])C.O.[NH2:21]N>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([CH3:10])=[N:21][NH:15][CH:17]=2)=[CH:4][CH:3]=1

参加物

4

反応物 3

HCID 24654Hydrazine hydrate (1:1)HCID 78373Dimethylformamide dimethyl acetalHCID 7363321-(4-Bromophenyl)propan-2-one

生成物 1

HCID 178434515HCID 178434515、化合物

反応条件

温度
90 °C

実験手順

To 4-bromophenylacetone (5.0 g, 23.5 mmol, 1.0 equiv) (Acros Organics 34216) was added N,N-dimethylformamide dimethyl acetal (11.3 ml, 84.6 mmol, 3.6 equiv) and the mixture was heated to 90° C. for 6 hours. The solvents were removed and the resulting gum was dissolved in ethanol (235 ml) with additional heating. Hydrazine hydrate (1.37 ml, 28.2 mmol, 1.2 equiv) was added and the mixture was heated to reflux for 15 hours. The solvents were removed under reduced pressure and the solid was triturated with dichloromethane to afford the title compound, 2.24 g (40%); LCMS (PS-A) Rt 2.87 min [M+H]+ 238. Further material could be isolated from the mother liquor.

後処理

  1. customThe solvents were removed
  2. dissolutionthe resulting gum was dissolved in ethanol (235 ml) with additional heating
  3. temperaturethe mixture was heated
  4. temperatureto reflux for 15 hours
  5. customThe solvents were removed under reduced pressure
  6. customthe solid was triturated with dichloromethane

出典と根拠

ORDレコード
ord-be9584ba2d8b4f1cb8d212bc767c796c
出典データセット
uspto-grants-2013_09
特許番号
US08541461B2

関連ノート

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