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Isopropanol → 5-chloro-1,3-dihydro-3-(2-oxopropyl)-1-(4-piperidinyl)-2H-benzimidazol-2-one hydrochloride

HRID 1729796
ノート
印刷プレビュー

反応式

HRID 1729796 の反応式
[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[N:6]([CH:13]3[CH2:18][CH2:17][N:16](C(OCC)=O)[CH2:15][CH2:14]3)[C:7](=[O:12])[N:8]([CH2:9][C:10]#[CH:11])[C:4]=2[CH:3]=1.[OH-].[K+].CC([OH:31])C>O>[ClH:1].[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[N:6]([CH:13]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[C:7](=[O:12])[N:8]([CH2:9][C:10](=[O:31])[CH3:11])[C:4]=2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3776IsopropanolHCID 14797Potassium HydroxideHCID 21500259ethyl 4-[5-chloro-1,3-dihydro-2-oxo-3-(2-propynyl)-2H-benzimidazol-1-yl]-1-piperidinecarboxylate

生成物 1

HCID 215002935-chloro-1,3-dihydro-3-(2-oxopropyl)-1-(4-piperidinyl)-2H-benzimidazol-2-one hydrochloride

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 14 parts of ethyl 4-[5-chloro-1,3-dihydro-2-oxo-3-(2-propynyl)-2H-benzimidazol-1-yl]-1-piperidinecarboxylate, 20 parts of potassium hydroxide, 128 parts of 2-propanol and 2.5 parts of water is stirred and refluxed overnight. After cooling, the solvent is evaporated and water is added to the residue. The product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The oily residue is converted into the hydrochloride salt in 2,2'-oxybispropane and 2-propanol. The salt is filtered off and crystallized from ethanol, yielding 5-chloro-1,3-dihydro-3-(2-oxopropyl)-1-(4-piperidinyl)-2H-benzimidazol-2-one hydrochloride.

後処理

  1. temperaturerefluxed overnight
  2. temperatureAfter cooling
  3. customthe solvent is evaporated
  4. additionwater is added to the residue
  5. extractionThe product is extracted with methylbenzene
  6. customThe extract is dried
  7. filtrationfiltered
  8. customevaporated
  9. filtrationThe salt is filtered off
  10. customcrystallized from ethanol

出典と根拠

ORDレコード
ord-43978ea7f44047f7a15504de23563666
出典データセット
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03989707

反応ノート

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