Ammonium Hydroxide → 9-Chloro-7-(2-chlorophenyl)-5H-pyrimido(5,4-d)(2)benzazepine

HRID 464202노트

반응식

HRID 464202 반응식
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[C:6]3[N:22]=[CH:21][N:20]=[CH:19][C:7]=3[CH2:8][N+:9]([O-])=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.P(Cl)(Cl)Cl.[OH-].[NH4+]>C(Cl)Cl>[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[C:6]3[N:22]=[CH:21][N:20]=[CH:19][C:7]=3[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 14923Ammonium HydroxideHCID 24387Phosphorus trichlorideHCID 132023249-Chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-6-oxide

생성물 1

HCID 1317369-Chloro-7-(2-chlorophenyl)-5H-pyrimido(5,4-d)(2)benzazepine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 0.5 g (1.3 mmol) of 9-chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-6-oxide and 1.0 ml (10 mmol) of phosphorous trichloride in 20 ml of methylene chloride was refluxed for 3 hr. The mixture was cooled, poured over ice, basified with ammonium hydroxide and extracted with methylene chloride. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and concentrated at reduced pressure. The residue crystallized upon the addition of ether to give colorless prisms, mp 121°-123° C.

후처리

  1. temperaturewas refluxed for 3 hr
  2. temperatureThe mixture was cooled
  3. additionpoured over ice
  4. extractionextracted with methylene chloride
  5. washThe methylene chloride solution was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated at reduced pressure
  8. customThe residue crystallized upon the addition of ether
  9. customto give colorless prisms, mp 121°-123° C.

출처 및 근거

ORD 기록
ord-8a5537dfc51744e4b595d49ac5ce8647
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04546183

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