Triphenylphosphine dichloride → 7,8-Dichloro-4-methylisoquinoline

HRID 1288483

반응식

HRID 1288483 반응식
[Cl:1][C:2]1[C:3](O)=[CH:4][CH:5]=[C:6]2[C:11]=1[CH:10]=[N:9][CH:8]=[C:7]2[CH3:12].[Cl:14]P(Cl)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>>[Cl:14][C:3]1[C:2]([Cl:1])=[C:11]2[C:6]([C:7]([CH3:12])=[CH:8][N:9]=[CH:10]2)=[CH:5][CH:4]=1

참가 물질

3

반응물 2

HCID 260420Triphenylphosphine dichlorideHCID 21393806HCID 21393806, 화합물

생성물 1

HCID 213938497,8-Dichloro-4-methylisoquinoline

실험 절차

8-Chloro-7-hydroxy-4-methylisoquinoline (0.04 mole) and dichlorotriphenylphosphorane (0.04 mole) are heated to 240° C. under a nitrogen atmosphere. After 4 hours, the mixture is allowed to cool and is partitioned between chloroform and concentrated hydrochloric acid. The acidic extract is washed with chloroform, basified and extracted with chloroform. The chloroform extract is washed with water, dried over sodium sulfate and evaporated to yield 7,8-dichloro-4-methylisoquinoline. The product is purified by chromatography on silica gel eluted with chloroform and finally by precipitation of the hydrochloride from ethanol-ether.

후처리

  1. temperatureto cool
  2. customis partitioned between chloroform and concentrated hydrochloric acid
  3. extractionThe acidic extract
  4. washis washed with chloroform
  5. extractionextracted with chloroform
  6. extractionThe chloroform extract
  7. washis washed with water
  8. dry with materialdried over sodium sulfate
  9. customevaporated

출처 및 근거

ORD 기록
ord-664b79f2620b49b5be4c8e1e52b49cab
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03988339

연결된 노트

불러오는 중…