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Isopropanol → 2-(4-piperidinylmethyl)-1-(2-thienylmethyl)-1H-benzimidazole

HRID 2309626
ノート
印刷プレビュー

反応式

HRID 2309626 の反応式
ClC1N=CN=C2C=1N=C(C)N2C.Cl.[S:14]1[CH:18]=[CH:17][CH:16]=[C:15]1[CH2:19][N:20]1[C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=2[N:22]=[C:21]1[CH2:29][CH:30]1[CH2:35][CH2:34][N:33](C(OCC)=O)[CH2:32][CH2:31]1.[OH-].[K+].CC(O)C>O>[NH:33]1[CH2:34][CH2:35][CH:30]([CH2:29][C:21]2[N:20]([CH2:19][C:15]3[S:14][CH:18]=[CH:17][CH:16]=3)[C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=3[N:22]=2)[CH2:31][CH2:32]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3776IsopropanolHCID 14797Potassium HydroxideHCID 108451716-chloro-8,9-dimethyl-9H-purineHCID 14012872HCID 14012872、化合物

生成物 1

HCID 140128742-(4-piperidinylmethyl)-1-(2-thienylmethyl)-1H-benzimidazole収率 49%

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

A mixture of 68 parts of ethyl 4-[[1-(2-thienylmethyl)-1H-benzimidazol-2-yl]methyl]-1-piperidinecarboxylate monohydrochloride, 95 parts of potassium hydroxide, 800 parts of 2-propanol and 10 parts of water was stirred and refluxed for 6 hours. The reaction mixture was evaporated and water was added to the residue. The product was extracted with methylbenzene. The extract was dried, filtered and evaporated. The residue was crystallized from 1,1'-oxybisethane. The product was filtered off and dried, yielding 27 parts (49%) of 2-(4-piperidinylmethyl)-1-(2-thienylmethyl)-1H-benzimidazole; mp. 117.4° C. (64).

後処理

  1. temperaturerefluxed for 6 hours
  2. customThe reaction mixture was evaporated
  3. additionwater was added to the residue
  4. extractionThe product was extracted with methylbenzene
  5. customThe extract was dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was crystallized from 1,1'-oxybisethane
  9. filtrationThe product was filtered off
  10. customdried

出典と根拠

ORDレコード
ord-c42cc502ad1a4def98db1b2cacc8aaad
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04695575

反応ノート

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