Phenyl glycidyl ether → HCID 19911532, 화합물

HRID 1533966노트

반응식

HRID 1533966 반응식
[O:1]([CH2:8][CH:9]1[CH2:11][O:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:12]([O:14][CH2:15][CH2:16][N:17]1[C:21]2=[N:22][CH:23]=[CH:24][CH:25]=[C:20]2[N:19]=[C:18]1[CH2:26][N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)[CH3:13]>CC(O)C>[CH2:12]([O:14][CH2:15][CH2:16][N:17]1[C:21]2=[N:22][CH:23]=[CH:24][CH:25]=[C:20]2[N:19]=[C:18]1[CH2:26][N:27]1[CH2:28][CH2:29][N:30]([CH2:11][CH:9]([CH2:8][O:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[OH:10])[CH2:31][CH2:32]1)[CH3:13]

참가 물질

4

반응물 2

HCID 31217Phenyl glycidyl etherHCID 19911564HCID 19911564, 화합물

생성물 1

HCID 19911532HCID 19911532, 화합물수율 31%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 1.65 parts of 2-(phenoxymethyl)oxirane, 8.9 parts of 3-(2-ethoxyethyl)-2-(1-piperazinylmethyl)-3H-imidazo[4,5-b]pyridine and 40 parts of 2-propanol was stirred for 20 hours at reflux temperature. The reaction mixture was evaporated and the residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2,2'-oxybispropane. The product was filtered off and dried, yielding 1.36 parts (31.0%) of 4-[[3-(2-ethoxyethyl)-3H-imidazo[4,5-b]pyridin-2-yl]methyl]-α-(phenoxymethyl)-1-piperazineethanol; mp. 102.5° C. (compound 118).

후처리

  1. temperatureat reflux temperature
  2. customThe reaction mixture was evaporated
  3. customthe residue was purified by column chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated
  7. customThe residue was crystallized from 2,2'-oxybispropane
  8. filtrationThe product was filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-079748b495934f93981da6d3a1f51f48
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05086056

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