2-(3-Methoxyprop-1-ynyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester → 2-(3-Methoxypropyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester

HRID 1753897ノート

反応式

HRID 1753897 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:6]([C:18]#[C:19][CH2:20][O:21][CH3:22])=[N:7][C:8]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)=[CH:9][C:10]=1[CH3:11])=[O:4]>CO.[Pd]>[CH3:1][O:2][C:3]([C:5]1[C:6]([CH2:18][CH2:19][CH2:20][O:21][CH3:22])=[N:7][C:8]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)=[CH:9][C:10]=1[CH3:11])=[O:4]

参加物

4

反応物 1

HCID 866643322-(3-Methoxyprop-1-ynyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester

生成物 1

HCID 866643332-(3-Methoxypropyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester収率 95%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a solution of 500 mg (1.64 mmol) 2-(3-methoxyprop-1-ynyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester in MeOH (30 ml) was added 170 mg 10%-Pd/C. The reaction solution was stirred under hydrogen atmosphere (balloon) at RT for 16 h. Then the mixture was filtered through celite and the filtrate was concentrated in vacuo. Purification of the residue by CC (hexane/EtOAc 9:1) provided 480 mg (1.55 mmol, 95%) 2-(3-methoxypropyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester.

後処理

  1. filtrationThen the mixture was filtered through celite
  2. concentrationthe filtrate was concentrated in vacuo
  3. customPurification of the residue by CC (hexane/EtOAc 9:1)

出典と根拠

ORDレコード
ord-26ec4c5d8d834e509ff945e3ce274493
出典データセット
uspto-grants-2015_10
特許番号
US09168259B2

反応ノート

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