Iodoethane → HCID 86739199、化合物

HRID 2296356ノート

反応式

HRID 2296356 の反応式
[CH3:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[CH:4]=[C:5]1[C:9]2=[N:10][C:11]3[CH:12]=[CH:13][C:14]([C:19]([OH:21])=[O:20])=[CH:15][C:16]=3[C:17](=[O:18])[N:8]2[CH2:7][CH2:6]1.[CH2:26](I)[CH3:27].C([O-])([O-])=O.[K+].[K+]>CN(C)C=O>[CH3:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[CH:4]=[C:5]1[C:9]2=[N:10][C:11]3[CH:12]=[CH:13][C:14]([C:19]([O:21][CH2:26][CH3:27])=[O:20])=[CH:15][C:16]=3[C:17](=[O:18])[N:8]2[CH2:7][CH2:6]1

参加物

5

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 53937337HCID 53937337、化合物

生成物 1

HCID 86739199HCID 86739199、化合物収率 83%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3-(2-methyl-benzylidene)-1,2,3,9-tetrahydro-9-oxo-pyrrolo[2,1-b]quinazoline-7-carboxylic acid (1 g) was reacted with ethyl iodide (0.93 g) and anhydrous K2CO3 (0.83 g) in dimethylformamide (10 ml) under stirring at room temperature for 16 hours. After dilution with ice water the precipitate was filtered and washed with water until neutral: crystallization from chloroform-ethanol gave 0.9 g of 3-(2-methyl-benzylidene)-1,2,3,9-tetrahydro-9-oxo-pyrrolo[2,1-b]quinazoline-7-carboxylic acid, ethyl ester, m.p. 184°-185° C.

後処理

  1. filtrationAfter dilution with ice water the precipitate was filtered
  2. washwashed with water until neutral:
  3. customcrystallization from chloroform-ethanol

出典と根拠

ORDレコード
ord-afc023879a744a9fbf1f313de4317374
出典データセット
uspto-grants-1984_01
特許番号
US04428952

反応ノート

読み込み中…