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

HRID 1288483

反応式

HRID 1288483 の反応式
[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

参加物

3

反応物 2

HCID 260420Triphenylphosphine dichlorideHCID 21393806HCID 21393806、化合物

生成物 1

HCID 213938497,8-Dichloro-4-methylisoquinoline

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-664b79f2620b49b5be4c8e1e52b49cab
出典データセット
uspto-grants-1976_10
特許番号
US03988339

関連ノート

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