Dimethylformamide diethylacetal → HCID 178484337、化合物

HRID 1931547ノート

反応式

HRID 1931547 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][N:10]=1)[C:5]([NH2:7])=[O:6].C(O[CH:14](OCC)[N:15]([CH3:17])[CH3:16])C>>[Br:1][C:2]1[CH:3]=[C:4]([C:5](/[N:7]=[CH:14]/[N:15]([CH3:17])[CH3:16])=[O:6])[CH:8]=[CH:9][N:10]=1

参加物

3

反応物 2

HCID 70913Dimethylformamide diethylacetalHCID 46254072-Bromoisonicotinamide

生成物 1

HCID 178484337HCID 178484337、化合物収率 98%

反応条件

温度
120 °C

実験手順

2-bromo-isonicotinamide (406.2 mg, 2.021 mmol) and N,N-dimethylformamide diethyl acetal (0.48 ml, 2.80 mmol) were combined and heated to 120° C. A short path distillation apparatus was used to collect the ethanol that was liberated during the reaction. The reaction mixture was a light orange solution that slowly turned darker until it had become a dark amber solution. After 1.5 hours, the reaction mixture was cooled to room temperature. The reaction mixture solidified upon cooling and was placed under high vacuum overnight to give the title compound (507.4 mg) as an off-white solid.

後処理

  1. distillationA short path distillation apparatus
  2. customto collect the ethanol that
  3. customwas liberated during the reaction
  4. temperaturethe reaction mixture was cooled to room temperature
  5. temperatureupon cooling
  6. customwas placed under high vacuum overnight

出典と根拠

ORDレコード
ord-4c08072b05fa48d28ec290fd86677c22
出典データセット
uspto-grants-2012_05
特許番号
US08188085B2

反応ノート

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