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

HRID 65926ノート

反応式

HRID 65926 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-351dad66b97341498fcf56c29e05b1a7
出典データセット
uspto-grants-1978_12
特許番号
US04129653

反応ノート

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