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

HRID 1769033ノート

反応式

HRID 1769033 の反応式
[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]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 57294109HCID 57294109、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 21881883Oxolane--water (1/1)溶媒HCID 22728543Water ethylacetate溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-17e85e41d4a7487383df2cb29d9ad0a1
出典データセット
uspto-grants-1995_01
特許番号
US05380731

反応ノート

読み込み中…