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

HRID 1900748노트

반응식

HRID 1900748 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

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.)).

후처리

  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

출처 및 근거

ORD 기록
ord-4bfa96b190d2450ab2312c1ced0a2472
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05576324

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