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

HRID 464534노트

반응식

HRID 464534 반응식
[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[C:6](=O)[C:7](=[CH:19]N(C)C)[CH2:8][N+:9]([O-:18])=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.Cl.[C:27]([NH2:30])(=[NH:29])[CH3:28].C[O-].[Na+]>CO.C(Cl)Cl.O>[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[C:6]3[N:30]=[C:27]([CH3:28])[N:29]=[CH:19][C:7]=3[CH2:8][N+:9]([O-:18])=[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

7

반응물 3

HCID 67170Acetamidine monohydrochlorideHCID 10942334Sodium MethoxideHCID 731657308-chloro-1-(2-chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one 2-oxide

생성물 1

HCID 132255119-Chloro-7-(2-chlorophenyl)-2-methyl-5H-pyrimido[5,4-d][2]-benzazepine-6-oxide

시약·촉매·용매 3

HCID 887Methanol용매2회HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 1 g (2.8 mmole) of 8-chloro-1-(2-chlorophenyl)-4-[(dimethylamino)methylene]-3,4-dihydro-5H-2-benzazepine-5-one-2-oxide, 1.0 g (11 mmole) of acetamidine hydrochloride and 2.0 ml (9.9 mmole) of a 4.46M methanol solution of sodium methoxide in a mixture of 20 ml of methanol and 20 ml of methylene chloride was stirred at room temperature for 2 hr. The mixture was diluted with water and extracted with methylene chloride. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and concentrated at reduced pressure to dryness. Recrystallization of the residue from a mixture of ether and methylene chloride gave a colorless solid, mp 215°-216° C.

후처리

  1. extractionextracted with methylene chloride
  2. washThe methylene chloride solution was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated at reduced pressure to dryness
  5. customRecrystallization of the residue
  6. additionfrom a mixture of ether and methylene chloride
  7. customgave a colorless solid, mp 215°-216° C.

출처 및 근거

ORD 기록
ord-aa67c9c24ee04ad7ac1c87b5852ba540
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04547581

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