Sodium Hydroxide → 2-[4-({[(6-Amino-5-chloro-2-methoxypyridin-3-yl)carbonyl]amino}-methyl)piperidine-1-yl]hexanoic acid

HRID 489809ノート

反応式

HRID 489809 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([C:10]([NH:12][CH2:13][CH:14]2[CH2:19][CH2:18][N:17]([CH:20]([CH2:26][CH2:27][CH2:28][CH3:29])[C:21]([O:23]CC)=[O:22])[CH2:16][CH2:15]2)=[O:11])=[CH:4][C:3]=1[Cl:30].[OH-].[Na+]>CO>[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([C:10]([NH:12][CH2:13][CH:14]2[CH2:19][CH2:18][N:17]([CH:20]([CH2:26][CH2:27][CH2:28][CH3:29])[C:21]([OH:23])=[O:22])[CH2:16][CH2:15]2)=[O:11])=[CH:4][C:3]=1[Cl:30]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22262611Ethyl 2-[4-({[(6-amino-5-chloro-2-methoxypyridin-3-yl)carbonyl]amino}methyl)piperidin-1-yl]hexanoate

生成物 1

HCID 222626632-[4-({[(6-Amino-5-chloro-2-methoxypyridin-3-yl)carbonyl]amino}-methyl)piperidine-1-yl]hexanoic acid収率 94.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of ethyl 2-[4-({[(6-amino-5-chloro-2-methoxypyridin-3-yl)carbonyl]amino}methyl)piperidin-1-yl]hexanoate (4.3 g, 9.75 mmol) in methanol (50 ml) was added 2N aqueous sodium hydroxide (9.8 ml, 19.5 mmol) and the mixture was refluxed for 12 h. After cooled to room temperature, concentrated in vacuo. The resultant solid was treated with 2N aqueous hydrochloric acid (19.5 ml) to afford white solid, which was collected by filtration, washed with water (50 ml) gave 3.8 g (94%) of the title compound as white powder.

後処理

  1. temperaturethe mixture was refluxed for 12 h
  2. concentrationconcentrated in vacuo
  3. additionThe resultant solid was treated with 2N aqueous hydrochloric acid (19.5 ml)
  4. customto afford white solid, which
  5. filtrationwas collected by filtration
  6. washwashed with water (50 ml)

出典と根拠

ORDレコード
ord-1162bcaf758c4476afe44aab01359071
出典データセット
uspto-grants-2005_12
特許番号
US06979690B2

反応ノート

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