Dimethylformamide → 12-formyl-2-methyl-3,4-dioxo-1,3,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine

HRID 1447415노트

반응식

HRID 1447415 반응식
P(Cl)(Cl)(Cl)=O.CN(C)[CH:8]=[O:9].[CH3:11][N:12]1[C:29](=[O:30])[C:28](=[O:31])[N:15]2[C:16]3[CH:27]=[CH:26][CH:25]=[CH:24][C:17]=3[CH2:18][N:19]3[CH:23]=[CH:22][CH:21]=[C:20]3[CH:14]2[CH2:13]1.C([O-])(=O)C.[Na+]>C(Cl)Cl.O>[CH:8]([C:23]1[N:19]2[C:20]([CH:14]3[CH2:13][N:12]([CH3:11])[C:29](=[O:30])[C:28](=[O:31])[N:15]3[C:16]3[CH:27]=[CH:26][CH:25]=[CH:24][C:17]=3[CH2:18]2)=[CH:21][CH:22]=1)=[O:9]

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 517045Sodium AcetateHCID 128377152-methyl-3,4-dioxo-1,2,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine

생성물 1

HCID 1283778412-formyl-2-methyl-3,4-dioxo-1,3,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

The starting material is prepared as follows: The mixture of 170 mg of phosphorus oxychloride and 100 ml of dimethylformamide is stirred at room temperature for 30 minutes, whereupon the solution of 281 mg of 2-methyl-3,4-dioxo-1,3,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine in 5 ml of methylene chloride is added dropwise. After 30 minutes, the mixture is refluxed for another 30 minutes and cooled to room temperature. It is combined with 1.5 g of sodium acetate in 5 ml of water, stirred for 30 minutes and the organic layer separated. It is washed with water, 5% aqueous sodium bicarbonate, dried, evaporated and the residue triturated with diethyl ether, to yield the 12-formyl-2-methyl-3,4-dioxo-1,3,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine melting at 300°-302°.

후처리

  1. customThe starting material is prepared
  2. additionis added dropwise
  3. temperaturethe mixture is refluxed for another 30 minutes
  4. customthe organic layer separated
  5. washIt is washed with water, 5% aqueous sodium bicarbonate
  6. customdried
  7. customevaporated
  8. customthe residue triturated with diethyl ether

출처 및 근거

ORD 기록
ord-a21d58ea44764e3aab68eb028fcda31d
출처 데이터셋
uspto-grants-1982_02
특허 번호
US04316900

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