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

HRID 1249363노트

반응식

HRID 1249363 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 23925Iron촉매HCID 1140Toluene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-213fe6b655e64d3aadd2ac6e91d16df5
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04631278

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