2-Chloro-5-methylaniline → HCID 178425400, 화합물

HRID 268242

반응식

HRID 268242 반응식
Cl.N([C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]3[N:21]=[CH:20][NH:19][C:17]3=2)[N:12]=[C:11]([CH3:22])[CH:10]=1)C1C=CC=CC=1.[Cl:23][C:24]1[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][C:25]=1[NH2:26]>C(O)C>[ClH:23].[Cl:23][C:24]1[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][C:25]=1[NH:26][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]3[N:21]=[CH:20][NH:19][C:17]3=2)[N:12]=[C:11]([CH3:22])[CH:10]=1

참가 물질

4

반응물 2

HCID 667702-Chloro-5-methylanilineHCID 178428198HCID 178428198, 화합물

생성물 1

HCID 178425400HCID 178425400, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 40 g. (0.184 m.) of the compound of Example I, C., 26.1 g. (0.184 m.) of 2-chloro-5-methylaniline and 500 ml. of ethanol was refluxed with stirring overnight. The reaction mixture was concentrated to dryness in vacuo, and the residue dissolved in 700 m. of MeOH. The insolubles were removed by filtration and the MeOh filtrate concentrated in vacuo to give 24 g. m.p. decomposes 315°-400°C. The crude product was triturated in 500 ml. of MeOH, then oven-dried (100°C) to give m.p. 332°-335°C.

후처리

  1. additionA mixture of 40 g
  2. concentrationThe reaction mixture was concentrated to dryness in vacuo
  3. dissolutionthe residue dissolved in 700 m
  4. customThe insolubles were removed by filtration
  5. concentrationthe MeOh filtrate concentrated in vacuo
  6. customto give 24 g
  7. customdecomposes 315°-400°C
  8. customThe crude product was triturated in 500 ml
  9. dry with materialof MeOH, then oven-dried (100°C)
  10. customto give m.p. 332°-335°C.

출처 및 근거

ORD 기록
ord-95bae04fd6d140d19cd347511d757773
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947434

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