Acetamide, N-(2-iodo-4-nitrophenyl)- → HCID 12335772, 화합물

HRID 259493노트

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HRID 259493 반응식
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]

참가 물질

3

반응물 1

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

생성물 1

HCID 12335772HCID 12335772, 화합물수율 116.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-ed28c9f05fce4175a7317fba8800442b
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04038320

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