Triethylamine → HCID 131724410, 화합물

HRID 2085735노트

반응식

HRID 2085735 반응식
[Si:1]([O:8][C:9]1[CH:10]=[CH:11][C:12](I)=[C:13]2[C:18]=1[N:17]=[CH:16][CH:15]=[CH:14]2)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[C:20]([O:24][C:25](=[O:28])[CH:26]=[CH2:27])([CH3:23])([CH3:22])[CH3:21].C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C(N(CC)CC)C>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(#N)C>[Si:1]([O:8][C:9]1[CH:10]=[CH:11][C:12](/[CH:27]=[CH:26]/[C:25]([O:24][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:28])=[C:13]2[C:18]=1[N:17]=[CH:16][CH:15]=[CH:14]2)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 15458tert-Butyl acrylateHCID 80271Tri-o-tolylphosphineHCID 68453232HCID 68453232, 화합물

생성물 1

HCID 131724410HCID 131724410, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 6342Acetonitrile용매

실험 절차

A mixture of Example 201B (5.00 g, 13.0 mmol), tert-butylacrylate (2.00 g, 15.6 mmol), palladium(II) acetate (175 mg, 0.78 mmol), and tri-o-tolylphosphine (951 mg, 3.12 mmol) in a sealed tube with triethylamine (8 mL) and acetonitrile (38 mL) was heated to 120° C. for 16 hours and then concentrated. The concentrate was purified by flash column chromatography on silica gel with 10-100% ethyl acetate/hexanes to provide the desired product.

후처리

  1. concentrationconcentrated
  2. customThe concentrate was purified by flash column chromatography on silica gel with 10-100% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-ab5a047fedc2456f9b1227c453520f5e
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06720338B2

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