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

HRID 323511

反応式

HRID 323511 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-97b2eacca48f4fa5a7262a1836bb0cc0
出典データセット
uspto-grants-2001_04
特許番号
US06211199B1

関連ノート

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