Sodium Hydroxide → 3-Methyl-2-{2-oxo-3-(4-(pyridin-4-ylmethoxy)benzyl)imidazolidin-1-yl}-butyric acid

HRID 1994306노트

반응식

HRID 1994306 반응식
[CH3:1][CH:2]([CH3:30])[CH:3]([N:9]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=3)=[CH:17][CH:16]=2)[C:10]1=[O:29])[C:4]([O:6]CC)=[O:5].[OH-].[Na+]>CO>[CH3:1][CH:2]([CH3:30])[CH:3]([N:9]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=3)=[CH:17][CH:16]=2)[C:10]1=[O:29])[C:4]([OH:6])=[O:5]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68538692Ethyl 3-methyl-2-{2-oxo-3-(4-(pyridin-4-ylmethoxy)benzyl)imidazolidin-1-yl}-butyrate

생성물 1

HCID 685396553-Methyl-2-{2-oxo-3-(4-(pyridin-4-ylmethoxy)benzyl)imidazolidin-1-yl}-butyric acid수율 81.8%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
0 °C

실험 절차

Ethyl 3-methyl-2-{2-oxo-3-(4-(pyridin-4-ylmethoxy)benzyl)imidazolidin-1-yl}-butyrate (45 mg; 0.11 mmol) was dissolved in methanol (1.5 ml) and cooled to 0° C. NaOH (1N, 5 ml) was added, and the mixture was allowed to warm to RT over the course of 3 h. The methanol was then removed under reduced pressure, and water (1.5 ml) and saturated NaH2PO4 solution (3 ml) were added to the residue. The solid was filtered off with suction and washed with water. Drying under reduced pressure at 60° C. resulted in 3-methyl-2-{2-oxo-3-(4-(pyridin-4-ylmethoxy)benzyl)imidazolidin-1-yl}-butyric acid (36 mg; 0.09 mmol). MS: 384.45 (M+H); Rt: 0.87 min (method: gradient 0 min 96% H2O (0.05% TFA) 2.0 min 95% acetonitrile, 95% acetonitrile to 2.4 min, 4% acetonitrile 2.45 min; flow rate 1 ml/min; column 0.4 μL (YMC J'sphere ODS H80 20X2 1.4μ); 30° C.)

후처리

  1. temperatureto warm to RT over the course of 3 h
  2. customThe methanol was then removed under reduced pressure, and water (1.5 ml) and saturated NaH2PO4 solution (3 ml)
  3. additionwere added to the residue
  4. filtrationThe solid was filtered off with suction
  5. washwashed with water
  6. customDrying under reduced pressure at 60° C.

출처 및 근거

ORD 기록
ord-34232875446548ccbef6be08589f5b58
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07652143B2

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