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

HRID 65930ノート

反応式

HRID 65930 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][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]

参加物

6

反応物 3

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

生成物 1

HCID 227563392,6-Dicarbethoxy-5-methyl-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 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°.

後処理

  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)

出典と根拠

ORDレコード
ord-5c0313cb4ad24413969ec2ff7cd2ced4
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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