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Lithium Hydroxide → 4-(3-Pyridylmethyloxymethyl)-2-phenylbenzoic acid

HRID 2121158
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반응식

HRID 2121158 반응식
C[O:2][C:3](=[O:25])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][CH2:12][C:13]2[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=2)=[CH:6][C:5]=1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[OH-].[Li+]>CO>[N:15]1[CH:16]=[CH:17][CH:18]=[C:13]([CH2:12][O:11][CH2:10][C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:25])=[O:2])=[C:5]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH:6]=2)[CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 540573764-(3-Pyridylmethyloxymethyl)-2-phenylbenzoic acid methyl ester

생성물 1

HCID 234361714-(3-Pyridylmethyloxymethyl)-2-phenylbenzoic acid수율 93.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution in methanol (5 mL) of [4-(3-pyridylmethyloxymethyl)-2-phenylbenzoic acid methyl ester (0.58 g), prepared as in Example 183A, was added saturated aqueous lithium hydroxide and the reaction mixture was stirred overnight at ambient temperature. The reaction mixture was warmed to 60° C. and stirred for 4 hours. The reaction mixture was concentrated in vacuo and the residue was taken up in water. The aqueous phase was taken to pH 5 with aqueous 3N HCl and extracted with chloroform. The organic phase was concentrated in vacuo to give 4-(3-pyridylmethyloxymethyl)-2-phenylbenzoic acid (0.52 g).

후처리

  1. temperatureThe reaction mixture was warmed to 60° C.
  2. stirringstirred for 4 hours
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. extractionextracted with chloroform
  5. concentrationThe organic phase was concentrated in vacuo

출처 및 근거

ORD 기록
ord-454e01ac0f8141d5a0214d53f659d1c9
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06693123B2

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