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

HRID 65930노트

반응식

HRID 65930 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][CH:10]([CH3:18])[N:9]2[CH:19]=1)([O:3][CH2:4][CH3:5])=[O:2].Cl[C:21]([O:23][CH2:24][CH3:25])=[O:22].[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:21]([O:23][CH2:24][CH3:25])=[O:22])[CH:10]([CH3:18])[N:9]2[CH:19]=1)([O:3][CH2:4][CH3:5])=[O:2]

참가 물질

6

반응물 3

HCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 227563592-Carbethoxy-5-methyl-5,6-dihydropyrrolo[1,2-c]quinazoline

생성물 1

HCID 227563392,6-Dicarbethoxy-5-methyl-5,6-dihydropyrrolo[1,2-c]quinazoline

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

A solution of the product of Example XXXVIII (3.0 g, 0.0117 m) and ethyl chloroformate (12.6 g, 0.117 m) in acetone (50 ml) and H2O (50 ml) was treated with NaOH (0.21 ml aq. 30%) and the mixture refluxed for 1 hr. The acetone was removed in vacuo and the aqueous residue cooled in ice-bath. A solid formed and this was filtered, washed with water, and dried in vacuo. The crude product (3.4 g) was crystallized from methanol (25 ml) to afford the desired product; m.p. 125°-127°.

후처리

  1. temperaturethe mixture refluxed for 1 hr
  2. customThe acetone was removed in vacuo
  3. temperaturethe aqueous residue cooled in ice-bath
  4. customA solid formed
  5. filtrationthis was filtered
  6. washwashed with water
  7. customdried in vacuo
  8. customThe crude product (3.4 g) was crystallized from methanol (25 ml)

출처 및 근거

ORD 기록
ord-5c0313cb4ad24413969ec2ff7cd2ced4
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04129653

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