Potassium thiocyanate → 5-Methyl-2-thiocyanato-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one

HRID 1900748ノート

反応式

HRID 1900748 の反応式
BrC[CH:3]1[O:17][C:6]2=[C:7]3[C:12](=[C:13]([CH3:15])[CH:14]=[C:5]2[CH2:4]1)[NH:11][C:10](=[O:16])[CH:9]=[CH:8]3.[S-:18][C:19]#[N:20].[K+]>CN(C)C=O>[CH3:15][C:13]1[CH:14]=[C:5]2[CH2:4][CH:3]([S:18][C:19]#[N:20])[O:17][C:6]2=[C:7]2[C:12]=1[NH:11][C:10](=[O:16])[CH:9]=[CH:8]2

参加物

4

反応物 2

HCID 516872Potassium thiocyanateHCID 233696452-Bromomethyl-5-methyl-2,3,6,7-tetrahydrofuro[2,3-f]quinoline-7-one

生成物 1

HCID 233697765-Methyl-2-thiocyanato-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one収率 88.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2-bromomethyl-5-methyl-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one (0.882 g), potassium thiocyanate (2.915 g) and dimethylformamide (40 ml) was stirred in a hot bath at 100° C. for 5 hours. The solvent was distilled off under reduced pressure. The residue was combined with water and extracted with chloroform. The chloroform extract liquid was washed with water, dried and condensed. The residue was crystallized from chloroform--n-hexane to obtain 0.683 g of the title compound as white powder (mp.: 227°-229° C. (dec.)).

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. extractionextracted with chloroform
  3. extractionThe chloroform extract liquid
  4. washwas washed with water
  5. customdried
  6. customcondensed
  7. customThe residue was crystallized from chloroform

出典と根拠

ORDレコード
ord-4bfa96b190d2450ab2312c1ced0a2472
出典データセット
uspto-grants-1996_11
特許番号
US05576324

反応ノート

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