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

HRID 489809노트

반응식

HRID 489809 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-1162bcaf758c4476afe44aab01359071
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06979690B2

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