Sodium Hydroxide → (1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(piperidin-4-yl)amine

HRID 323511노트

반응식

HRID 323511 반응식
[OH:1][CH2:2][CH2:3][N:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=[C:5]1[NH:13][CH:14]1[CH2:19][CH2:18][N:17](C(OCC)=O)[CH2:16][CH2:15]1.[OH-].[Na+]>C(O)(C)C.O>[OH:1][CH2:2][CH2:3][N:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=[C:5]1[NH:13][CH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 22009172(1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(1-(ethoxycarbonyl)piperidin-4-yl)amine

생성물 1

HCID 22009128(1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(piperidin-4-yl)amine

시약·촉매·용매 2

HCID 962Water용매2회HCID 3776Isopropanol용매

실험 절차

Combine (1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(1-(ethoxycarbonyl)piperidin-4-yl)amine (5.0 mmol) and sodium hydroxide (2.0 g) in isopropanol (20 mL) and water (0.1 mL). Heat to reflux. After 36 hours, cool and evaporate the reaction mixture in vacuo to give a residue. Combine the residue and water. Extract the diluted residue three times with ethyl acetate. Combine the organic layers and extract with brine, dry over Na2SO4, filter, and evaporate in vacuo to give the title compound.

후처리

  1. temperatureHeat to reflux
  2. temperaturecool
  3. customevaporate the reaction mixture in vacuo
  4. customto give a residue
  5. extractionExtract the diluted residue three times with ethyl acetate
  6. extractionextract with brine
  7. dry with materialdry over Na2SO4
  8. filtrationfilter
  9. customevaporate in vacuo

출처 및 근거

ORD 기록
ord-97b2eacca48f4fa5a7262a1836bb0cc0
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211199B1

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