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Water → HCID 10411519, 화합물

HRID 898924
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HRID 898924 반응식
[CH2:1]([N:3]([CH2:27][C:28]1[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=1)[C:4](=[O:26])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][O:15][C:16]2[CH:25]=[CH:24][CH:23]=[CH:22][C:17]=2[C:18]([O:20]C)=[O:19])=[CH:9][CH:8]=1)[CH3:2].O.[OH-].[Li+]>C1COCC1>[CH2:1]([N:3]([CH2:27][C:28]1[CH:29]=[CH:30][C:31]([F:34])=[CH:32][CH:33]=1)[C:4](=[O:26])[CH2:5][O:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:13][CH2:14][O:15][C:16]2[CH:25]=[CH:24][CH:23]=[CH:22][C:17]=2[C:18]([OH:20])=[O:19])=[CH:11][CH:12]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 69258837HCID 69258837, 화합물

생성물 1

HCID 10411519HCID 10411519, 화합물수율 90.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Methyl 2-[2-(4-{2-[ethyl(4-fluorobenzyl)amino]-2-oxoethoxy}phenyl)ethoxy]-benzoate (0.223 g, 0.479 mmol) was dissolved in a mixture of THF (freshly distilled)/water (2/1, 3 ml), lithium hydroxide (0.229 g, 0.958 mmol) was added. The reaction was performed in a single node microwave oven (5 min, 150 deg). THF was removed by evaporation. Water was added (10 ml) and the basic water phase was washed with diethyl ether (2×10 ml). Addition of HCl (2 ml, 1 M, pH 1). The water phase was extracted with two portions of DCM (20 ml), the organic phase was dried (MgSO4) and the solvent was removed by evaporation to give 0.196 g of 2-[2-(4-{2-[ethyl(4-fluorobenzyl)amino]-2-oxoethoxy}phenyl)ethoxy]benzoic acid (yield 90.6%).

후처리

  1. additionwas added
  2. customThe reaction was performed in a single node microwave oven
  3. custom(5 min, 150 deg)
  4. customTHF was removed by evaporation
  5. additionWater was added (10 ml)
  6. washthe basic water phase was washed with diethyl ether (2×10 ml)
  7. additionAddition of HCl (2 ml, 1 M, pH 1)
  8. extractionThe water phase was extracted with two portions of DCM (20 ml)
  9. dry with materialthe organic phase was dried (MgSO4)
  10. customthe solvent was removed by evaporation

출처 및 근거

ORD 기록
ord-9537041078984df2abef81b77834b723
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07351858B2

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