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HCID 13105519, 화합물 → 1-(2-(Piperazin-1-YL)ethyl)-1,3-dihydro-2H-benzo[D]imidazol-2-one

HRID 1413494
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HRID 1413494 반응식
C1(C[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][N:16]3[C:20]4[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=4[NH:18][C:17]3=[O:25])[CH2:10][CH2:9]2)C=CC=CC=1.[H][H]>[Pd].CO>[N:11]1([CH2:14][CH2:15][N:16]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[NH:18][C:17]2=[O:25])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 13105519HCID 13105519, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 131056241-(2-(Piperazin-1-YL)ethyl)-1,3-dihydro-2H-benzo[D]imidazol-2-one

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 79 parts of 1,3-dihydro-1-{2-[4-(phenylmethyl)-1-piperazinyl]ethyl}-2H-benzimidazol-2-one and 320 parts of methanol is hydrogenated at normal pressure and at room temperature with 10 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The oily residue is alkalized with ammonium hydroxide and a small amount of water is added. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The oily residue solidifies on triturating in 4-methyl-2-pentanone. The product is filtered off and dried, yielding 1,3-dihydro-1-[2-(1-piperazinyl)ethyl}-2H-benzimidazol-2-one; mp. 122.6° C.

후처리

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. additiona small amount of water is added
  4. extractionThe product is extracted with trichloromethane
  5. customThe extract is dried
  6. filtrationfiltered
  7. customevaporated
  8. customon triturating in 4-methyl-2-pentanone
  9. filtrationThe product is filtered off
  10. customdried

출처 및 근거

ORD 기록
ord-8d50ddbee5594813bb2741b3f2754e44
출처 데이터셋
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04250176

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