Dimethylformamide → HCID 22440208、化合物

HRID 963256

反応式

HRID 963256 の反応式
Cl[C:2]1[C:11]2[CH:10]=[C:9]([OH:12])[CH:8]=[CH:7][C:6]=2[N:5]=[C:4]2[C:13]3[C:18]([C:19](=[O:20])[C:3]=12)=[CH:17][CH:16]=[CH:15][CH:14]=3.C(=O)([O-])[O-].[Li+].[Li+].Cl.[CH2:28]([N:30]([CH2:34]C)[CH2:31][CH2:32][SH:33])C.CN(C)C=O>O>[CH3:28][N:30]([CH2:31][CH2:32][S:33][C:2]1[C:11]2[CH:10]=[C:9]([OH:12])[CH:8]=[CH:7][C:6]=2[N:5]=[C:4]2[C:13]3[C:18]([C:19](=[O:20])[C:3]=12)=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH3:34]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11125Lithium CarbonateHCID 16031Ethanethiol, 2-(diethylamino)-, hydrochloride (1:1)HCID 1908181510-chloro-8-hydroxy-11H-indeno[1,2-b]quinolin-11-one

生成物 1

HCID 22440208HCID 22440208、化合物収率 63.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A mixture of 400 mg (1.4 mmol) of 10-chloro-8-hydroxy-11H-indeno[1,2-b]quinolin-11-one, 629 mg (8.5 mmol) of lithium carbonate, 963 mg (5.7 mmol) of 2-diethylaminoethanethiol hydrochloride and 8 ml of N,N-dimethylformamide was stirred for 5 hours with heating at 90° C. After completion of the reaction, the reaction mixture was added to water, and precipitated crystals were collected by filteration. The crystals were recrystallized from ethanol, giving 310 mg of the title compound (yield: 57.7%). The property values are shown in Table 1.

後処理

  1. customAfter completion of the reaction
  2. customprecipitated crystals
  3. customwere collected by filteration
  4. customThe crystals were recrystallized from ethanol

出典と根拠

ORDレコード
ord-f77d3e454a19410ba31af60dc53a8981
出典データセット
uspto-grants-1998_06
特許番号
US05763453

関連ノート

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