Methanol → HCID 67027121、化合物

HRID 2065875ノート

反応式

HRID 2065875 の反応式
[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]

参加物

5

反応物 2

HCID 887MethanolHCID 67026987HCID 67026987、化合物

生成物 1

HCID 67027121HCID 67027121、化合物収率 96.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 5,6-divinyl-nicotinic acid tert-butyl ester (890 mg, 3.8 mmol) in THF (20 mL) containing some MeOH, 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.

後処理

  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)

出典と根拠

ORDレコード
ord-1f42c4b905bb49f7b8541604e569f3bb
出典データセット
uspto-grants-2012_10
特許番号
US08288554B2

反応ノート

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