1-Isoquinolinamine → STK019752

HRID 1446809노트

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HRID 1446809 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.[C:12]1([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:17]=[CH:16][C:15]([CH:18]([C:20](C(Br)C2C=CC(C3C=CC=CC=3)=CC=2)=O)Br)=[CH:14][CH:13]=1>C(Cl)(Cl)Cl>[C:12]1([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:13]=[CH:14][C:15]([C:18]2[N:1]=[C:2]3[C:11]4[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=4)[CH:5]=[CH:4][N:3]3[CH:20]=2)=[CH:16][CH:17]=1

참가 물질

4

반응물 2

HCID 737421-IsoquinolinamineHCID 86737811HCID 86737811, 화합물

생성물 1

HCID 1338745STK019752

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
100 °C

실험 절차

A solution of 4.32 g. (0.03 mole) of 1-amino-isoquinoline and 8.25 g. (0.03 mole) of [(1,1'-biphenyl)-4-yl]-bromomethyl-ketone in 100 ml. of chloroform was heated on a boiling water bath for about 10 minutes until a precipitate separated. The solvent was distilled off at atmospheric pressure and the residue was heated under vacuum for 30 minutes at 100° C. It was subsequently taken up with 50 ml of water and the resulting solution was made alkaline by means of 70 ml. of aqueous 10% sodium hydroxide. After extracting with 500 ml. of methylene chloride and evaporating the solvent, a residue was obtained which was re-crystallized from ethylene glycol monomethylether. Yield 3.0 g. M.p. 221°-22° C.

후처리

  1. customseparated
  2. distillationThe solvent was distilled off at atmospheric pressure
  3. extractionAfter extracting with 500 ml
  4. customof methylene chloride and evaporating the solvent
  5. customa residue was obtained which
  6. customwas re-crystallized from ethylene glycol monomethylether

출처 및 근거

ORD 기록
ord-9b94ea4a78b34cc6afbf3ba2be2499b5
출처 데이터셋
uspto-grants-1982_02
특허 번호
US04313950

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