Sodium Hydroxide → 5-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one

HRID 2417795

反応式

HRID 2417795 の反応式
C([N:6]1[CH2:11][CH2:10][CH:9]([N:12]2[C:16]3[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:15]=3[NH:14][C:13]2=[O:22])[CH2:8][CH2:7]1)(OCC)=O.[OH-].[Na+].[Cl-].[NH4+]>O>[Cl:21][C:19]1[CH:18]=[CH:17][C:16]2[N:12]([CH:9]3[CH2:8][CH2:7][NH:6][CH2:11][CH2:10]3)[C:13](=[O:22])[NH:14][C:15]=2[CH:20]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 104610Ethyl 4-(5-chloro-2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinecarboxylate

生成物 1

HCID 1046075-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 22.3 g of 1-carbethoxy-4-(5-chlorobenzimidazol-2-on-1-yl)-piperidine, 13 g of 50% strength sodium hydroxide solution and 90 ml of water was boiled under reflux for 24 hours. After the mixture had been cooled, the solution was stirred with 8.5 g of ammonium chloride for 30 minutes and extracted with chloroform, and the undissolved material was filtered off and discarded. The chloroform solution was dried and evaporated. The product crystallized, and has a melting point of 220° C.

後処理

  1. temperatureunder reflux for 24 hours
  2. temperatureAfter the mixture had been cooled
  3. extractionextracted with chloroform
  4. filtrationthe undissolved material was filtered off
  5. dry with materialThe chloroform solution was dried
  6. customevaporated
  7. customThe product crystallized

出典と根拠

ORDレコード
ord-81f7d53e494e42f0a6b69705f54f78bd
出典データセット
uspto-grants-1984_09
特許番号
US04470989

関連ノート

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