Formamidine acetate → 9-Chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-6-oxide

HRID 464201

반응식

HRID 464201 반응식
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[C:6](=O)[C:7](=[CH:18]N(C)C)[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.C(O)(=[O:27])C.[CH:29]([NH2:31])=[NH:30]>C(N)=N>[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[C:6]3[N:31]=[CH:29][N:30]=[CH:18][C:7]=3[CH2:8][N+:9]([O-:27])=[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

4

반응물 2

HCID 160693Formamidine acetateHCID 536569248-Chloro-1-(2-chlorophenyl)-4-dimethylaminomethylidene-3,4-dihydro-2-benzazepin-5-one

생성물 1

HCID 132023249-Chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-6-oxide

시약·촉매·용매 1

HCID 68047Formamidine용매

실험 절차

A mixture of 0.4 g (1.1 mmol) of 8-chloro-1-(2-chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one and 1.0 g (9.6 mmol) of formamidine acetate in 20 ml of formamidine was heated on a steam bath for 7 hr. The mixture was poured over ice 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 was triturated with ether to give an off-white solid, mp 215°-217° C.

후처리

  1. temperaturewas heated on a steam bath for 7 hr
  2. additionThe mixture was poured over ice
  3. extractionextracted with methylene chloride
  4. washThe methylene chloride solution was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated at reduced pressure
  7. customThe residue was triturated with ether
  8. customto give an off-white solid, mp 215°-217° C.

출처 및 근거

ORD 기록
ord-948dd322c1d840f3a9fea18204c339d9
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04546183

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