Methanol → HCID 67027121, 화합물

HRID 1908767노트

반응식

HRID 1908767 반응식
[C:1]([O:5][C:6](=[O:17])[C:7]1[CH:12]=[C:11]([CH:13]=[CH2:14])[C:10]([CH:15]=[CH2:16])=[N:9][CH:8]=1)([CH3:4])([CH3:3])[CH3:2].CO>C1COCC1.[Pd]>[C:1]([O:5][C:6](=[O:17])[C:7]1[CH:12]=[C:11]([CH2:13][CH3:14])[C:10]([CH2:15][CH3:16])=[N:9][CH:8]=1)([CH3:3])([CH3:4])[CH3:2]

참가 물질

5

반응물 2

HCID 887MethanolHCID 67026987HCID 67026987, 화합물

생성물 1

HCID 67027121HCID 67027121, 화합물수율 96.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5,6-divinyl-nicotinic acid tert-butyl ester (890 mg, 3.8 mmol) in THF (20 mL) containing some methanol, Pd/C (100 mg, 10% Pd) is added and the mixture is stirred under 1 atm of H2 at rt for 3 h. The catalyst is filtered off and the filtrate is evaporated. The remaining residue is purified by FC (SiO2, EA-heptane) to give 5,6-diethyl-nicotinic acid tert-butyl ester (860 mg) as an oil; LC-MS: tR=0.79 min, [M+1]+=236.14.

후처리

  1. additionis added
  2. filtrationThe catalyst is filtered off
  3. customthe filtrate is evaporated
  4. customThe remaining residue is purified by FC (SiO2, EA-heptane)

출처 및 근거

ORD 기록
ord-889a8acac4024f0988e88ea7985ac46a
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08598208B2

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