Triphenylphosphine → ((3-Chlorothieno[3,2-b]pyridin-5-yl)methyl)triphenylphosphonium chloride

HRID 2259486ノート

反応式

HRID 2259486 の反応式
[Cl:1][C:2]1[C:6]2=[N:7][C:8]([CH2:11]Cl)=[CH:9][CH:10]=[C:5]2[S:4][CH:3]=1.[P:13]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>CC#N>[Cl-:1].[Cl:1][C:2]1[C:6]2=[N:7][C:8]([CH2:11][P+:13]([C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)=[CH:9][CH:10]=[C:5]2[S:4][CH:3]=1

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 190028563-Chloro-5-(chloromethyl)thieno[3,2-b]-pyridine

生成物 1

HCID 88252540((3-Chlorothieno[3,2-b]pyridin-5-yl)methyl)triphenylphosphonium chloride収率 159%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 3-chloro-5-(chloromethyl)thieno[3,2-b]-pyridine (1.2 g, 5.5 mmol) in CH3CN (20 mL) was added P(Ph)3 (2.88 g, 11 mmol). The mixture was refluxed for 20 hr. and was then evaporated to dryness. Et2O (8 mL) was added. The mixture was stirred vigorously and the crystalline salt was filtered and washed with more Et2O to give. 2.1 g (81%) of the title compound.

後処理

  1. temperatureThe mixture was refluxed for 20 hr
  2. customand was then evaporated to dryness
  3. additionEt2O (8 mL) was added
  4. filtrationthe crystalline salt was filtered
  5. washwashed with more Et2O
  6. customto give

出典と根拠

ORDレコード
ord-e9627dcfb2e64002af7c87094f894747
出典データセット
uspto-grants-1995_12
特許番号
US05472964

反応ノート

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