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 1039783ノート

反応式

HRID 1039783 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-a2c9542b2c5c45eeb29bad340473e67b
出典データセット
uspto-grants-2013_10
特許番号
US08552200B2

反応ノート

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