Methane → Ethyl 4-(5-chloro-2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinecarboxylate

HRID 2417794ノート

反応式

HRID 2417794 の反応式
[C:1]([N:6]1[CH2:11][CH2:10][CH:9]([NH:12][C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[NH2:20])[CH2:8][CH2:7]1)([O:3][CH2:4][CH3:5])=[O:2].N[C:22](N)=[O:23].C>C1(C)C=CC=CC=1>[C:1]([N:6]1[CH2:7][CH2:8][CH:9]([N:12]2[C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[NH:20][C:22]2=[O:23])[CH2:10][CH2:11]1)([O:3][CH2:4][CH3:5])=[O:2]

参加物

5

反応物 3

HCID 297MethaneHCID 1176UreaHCID 104609Ethyl 4-(2-amino-4-chloroanilino)piperidine-1-carboxylate

生成物 1

HCID 104610Ethyl 4-(5-chloro-2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinecarboxylate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 24.7 g of 1-carbethoxy-4-(2-amino-4-chloroanilino)-piperidine and 7.2 g of urea was heated to 160°-180° C. for 3.5 hours. The melt was taken up in 250 ml of toluene and heated, while stirring, until everything had dissolved. The solution was clarified with active charcoal, filtered and concentrated to 50 ml. The product was precipitated with diisopropyl ether. Melting point: 160° C.

後処理

  1. temperaturewas heated to 160°-180° C. for 3.5 hours
  2. temperatureheated
  3. dissolutionhad dissolved
  4. filtrationfiltered
  5. concentrationconcentrated to 50 ml
  6. customThe product was precipitated with diisopropyl ether

出典と根拠

ORDレコード
ord-ce47b2e418934eda94a0f219f6f3ac23
出典データセット
uspto-grants-1984_09
特許番号
US04470989

反応ノート

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