Ethyl chloroformate → 2,6-Dicarbethoxy-5,6-dihydropyrrolo[1,2-c]quinazoline

HRID 65926노트

반응식

HRID 65926 반응식
[C:1]([C:6]1[CH:7]=[C:8]2[C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[NH:11][CH2:10][N:9]2[CH:18]=1)([O:3][CH2:4][CH3:5])=[O:2].Cl[C:20]([O:22][CH2:23][CH3:24])=[O:21].[OH-].[Na+]>CC(C)=O.O>[C:1]([C:6]1[CH:7]=[C:8]2[C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:11]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:10][N:9]2[CH:18]=1)([O:3][CH2:4][CH3:5])=[O:2]

참가 물질

6

반응물 3

HCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 227563502-Carbethoxy-5,6-dihydropyrrolo[1,2-c]quinazoline

생성물 1

HCID 125700262,6-Dicarbethoxy-5,6-dihydropyrrolo[1,2-c]quinazoline

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

A solution of the product of Example IV (1.2 g, 0.005 m) and ethyl chloroformate (6.0 g, 0.0553 m) in acetone (20 ml) and H2O (50 ml) was treated with NaOH (0.1 ml aq. 30%) and the mixture stirred at room temperature for 15 min. The acetone was removed in vacuo and the aqueous residue cooled in an ice-bath. A solid formed and this was filtered, washed with water, and dried in vacuo. The crude product (1.0 g) was crystallized from methanol to afford the desired product; m.p. 80°-82° C.

후처리

  1. customThe acetone was removed in vacuo
  2. temperaturethe aqueous residue cooled in an ice-bath
  3. customA solid formed
  4. filtrationthis was filtered
  5. washwashed with water
  6. customdried in vacuo
  7. customThe crude product (1.0 g) was crystallized from methanol

출처 및 근거

ORD 기록
ord-351dad66b97341498fcf56c29e05b1a7
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04129653

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