Acetamide, N-(2-iodo-4-nitrophenyl)- → HCID 12335772、化合物

HRID 259493ノート

反応式

HRID 259493 の反応式
I[C:2]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:3]=1[NH:4][C:5](=[O:7])[CH3:6]>CN(C=O)C>[C:5]([NH:4][C:3]1[CH:8]=[CH:9][C:10]([N+:12]([O-:14])=[O:13])=[CH:11][C:2]=1[C:2]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:3]=1[NH:4][C:5](=[O:7])[CH3:6])(=[O:7])[CH3:6]

参加物

3

反応物 1

HCID 4400707Acetamide, N-(2-iodo-4-nitrophenyl)-

生成物 1

HCID 12335772HCID 12335772、化合物収率 116.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

A mixture of 2'-iodo-4'-nitroacetanilide (II) (50.02 g, 0.164 mole), copper-bronze (87.9 g) and N,N'-dimethylformamide (350 ml) was stirred and heated at 150° C. under nitrogen for 1 hour and filtered. The filter cake was washed with tetrahydrofuran, and the combined filtrate and washings were concentrated under vacuum to 100 ml and poured, with stirring, into 1200 ml of concentrated ammonium hydroxide. The resultant precipitate was filtered, washed with water, and dried at 100° C. and 1 mm Hg to yield 34.1 g (58 %) of 2,2'-bis-(acetamido)-5,5'-dinitrobiphenyl. An analytical sample, m.p. 263°- 265° C., was obtained by recrystallization from ethanol.

後処理

  1. filtrationfiltered
  2. washThe filter cake was washed with tetrahydrofuran
  3. concentrationthe combined filtrate and washings were concentrated under vacuum to 100 ml
  4. additionpoured
  5. stirringwith stirring, into 1200 ml of concentrated ammonium hydroxide
  6. filtrationThe resultant precipitate was filtered
  7. washwashed with water
  8. customdried at 100° C.

出典と根拠

ORDレコード
ord-ed28c9f05fce4175a7317fba8800442b
出典データセット
uspto-grants-1977_07
特許番号
US04038320

反応ノート

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