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

HRID 2309626
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HRID 2309626 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c42cc502ad1a4def98db1b2cacc8aaad
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04695575

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