2-Chloro-5-methylaniline → HCID 178425400、化合物

HRID 268242

反応式

HRID 268242 の反応式
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

参加物

4

反応物 2

HCID 667702-Chloro-5-methylanilineHCID 178428198HCID 178428198、化合物

生成物 1

HCID 178425400HCID 178425400、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-95bae04fd6d140d19cd347511d757773
出典データセット
uspto-grants-1976_03
特許番号
US03947434

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