Tributylstannane → HCID 20061023、化合物

HRID 1085149ノート

反応式

HRID 1085149 の反応式
[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([C:13]#[N:14])=[CH:9][CH:8]=2)[C:5]([CH3:15])=[N:4][C:3]=1I.C([SnH](CCCC)CCCC)CCC.[F-].[K+].C1C[O:35][CH2:34]C1>>[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([C:13]#[N:14])=[CH:9][CH:8]=2)[C:5]([CH3:15])=[N:4][C:3]=1[CH:34]=[O:35]

参加物

5

反応物 4

HCID 5948TributylstannaneHCID 8028Tetrahydrofuran2 回HCID 522689Potassium FluorideHCID 20060989HCID 20060989、化合物

生成物 1

HCID 20061023HCID 20061023、化合物

反応条件

温度
50 °C

実験手順

A solution of the product from (b) (1.03 g, 3 mmol) and tetrakis (triphenylphosphine)palladium (0.3 g) in THF (70 ml) was installed under an atmosphere of carbon monoxide and heated to 50° C. Tributyltin hydride (0.96 g, 3.3 mmol) in THF (40 ml) was instilled by motor-driven syringe over 4.5 hours. After an additional 0.5 hours the mixture was stirred with 100 ml of 10% potassium fluoride solution for 15 minutes, then extracted twice with dichloromethane. The organic layers were dried over magnesium sulphate and evaporated to an orange solid.

後処理

  1. extractionextracted twice with dichloromethane
  2. dry with materialThe organic layers were dried over magnesium sulphate
  3. customevaporated to an orange solid

出典と根拠

ORDレコード
ord-8515b0802c154cb3bfff6ca4b2bbdeb1
出典データセット
uspto-grants-1991_04
特許番号
US05008263

反応ノート

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