Tributylstannane → HCID 20061023, 화합물

HRID 1085149노트

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HRID 1085149 반응식
[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]

참가 물질

5

반응물 4

HCID 5948TributylstannaneHCID 8028Tetrahydrofuran2회HCID 522689Potassium FluorideHCID 20060989HCID 20060989, 화합물

생성물 1

HCID 20061023HCID 20061023, 화합물

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온도
50 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-8515b0802c154cb3bfff6ca4b2bbdeb1
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05008263

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