Lithium Hydroxide → 1-[[(2-Ethoxy)ethyl]-1H-benzimidazol-2-yl][1-(carboxy methoxy ethyl)-4-piperidinyl]methanone

HRID 1769033노트

반응식

HRID 1769033 반응식
[CH3:1][CH2:2][O:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]=[C:7]1[C:15]([CH:17]1[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][O:25][CH2:26][C:27]([O:29]C)=[O:28])[CH2:19][CH2:18]1)=[O:16].[OH-].[Li+]>O1CCCC1.O.C(OCC)(=O)C.O>[CH3:1][CH2:2][O:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]=[C:7]1[C:15]([CH:17]1[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][O:25][CH2:26][C:27]([OH:29])=[O:28])[CH2:19][CH2:18]1)=[O:16]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 57294109HCID 57294109, 화합물

생성물 1

HCID 1317188291-[[(2-Ethoxy)ethyl]-1H-benzimidazol-2-yl][1-(carboxy methoxy ethyl)-4-piperidinyl]methanone

시약·촉매·용매 2

HCID 21881883Oxolane--water (1/1)용매HCID 22728543Water ethylacetate용매

반응 조건

온도
60 °C

실험 절차

Dissolve 1-[[(2-ethoxy)ethyl]-1H-benzimidazol-2-yl][1-(carbomethoxy methoxy ethyl)-4-piperidinyl]methanone (0.9 g, 2.15 mmol) in tetrahydrofuran/water (20 mL, 1/1). Add lithium hydroxide monohydroate (932 mg, 8.5 mmol). Seal the flask and warm to 60° C. for 3 hours. Dilute with ethyl acetate/water, acidify and separate the organic phase. Dry (MgSO4), evaporate the solvent in vacuo, and purify by ion-exchange chromatography to give the title compound.

후처리

  1. customSeal the flask
  2. customseparate the organic phase
  3. dry with materialDry (MgSO4)
  4. customevaporate the solvent in vacuo
  5. custompurify by ion-exchange chromatography

출처 및 근거

ORD 기록
ord-17e85e41d4a7487383df2cb29d9ad0a1
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05380731

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