Ammonium Chloride → alpha-(4-Amino-2-chlorophenyl)-4-chloro-alpha-methylbenzeneacetonitrile

HRID 1249363ノート

反応式

HRID 1249363 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:12]2[CH:17]=[CH:16][C:15]([N+:18]([O-])=O)=[CH:14][C:13]=2[Cl:21])([CH3:11])[C:9]#[N:10])=[CH:4][CH:3]=1.[Cl-].[NH4+]>[Fe].CC1C=CC=CC=1>[NH2:18][C:15]1[CH:16]=[CH:17][C:12]([C:8]([CH3:11])([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[C:9]#[N:10])=[C:13]([Cl:21])[CH:14]=1

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 137703554-Chloro-alpha-(2-chloro-4-nitrophenyl)-alpha-methylbenzeneacetonitrile

生成物 1

HCID 13770357alpha-(4-Amino-2-chlorophenyl)-4-chloro-alpha-methylbenzeneacetonitrile

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 1140Toluene溶媒

実験手順

A mixture of 20 parts of 4-chloro-α-(2-chloro-4-nitrophenyl)-α-methylbenzeneacetonitrile, 7 parts of iron powder, 250 parts of ammonium chloride solution 0.78N and 200 parts of methylbenzene was stirred and refluxed for 3 hours. The reaction mixture was filtered hot. The aqueous phase was separated and washed with methylbenzene. The combined organic layers were washed successively with water, sodium hydrogen carbonate solution and again with water, dried and evaporated. The residue was washed with 1,1'-oxybisethane and dried, yielding 10 parts of α-(4-amino-2-chlorophenyl)-4-chloro-α-methylbenzeneacetonitrile; mp. 135.2° C. (intermediate 24).

後処理

  1. temperaturerefluxed for 3 hours
  2. filtrationThe reaction mixture was filtered hot
  3. customThe aqueous phase was separated
  4. washwashed with methylbenzene
  5. washThe combined organic layers were washed successively with water, sodium hydrogen carbonate solution and again with water
  6. customdried
  7. customevaporated
  8. washThe residue was washed with 1,1'-oxybisethane
  9. customdried

出典と根拠

ORDレコード
ord-213fe6b655e64d3aadd2ac6e91d16df5
出典データセット
uspto-grants-1986_12
特許番号
US04631278

反応ノート

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