Benzyl Chloride → HCID 67922776, 화합물

HRID 1110390노트

반응식

HRID 1110390 반응식
[CH3:1][O:2][C@H:3]1[C@@H:8]([NH:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6][N:5]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:4]1.Cl[CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(=O)([O-])[O-].[Na+].[Na+]>CC1C=CC=CC=1>[C:11]1([CH2:10][N:9]([CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C@H:8]2[CH2:7][CH2:6][N:5]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:4][C@H:3]2[O:2][CH3:1])[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

5

반응물 3

HCID 7503Benzyl ChlorideHCID 10340Sodium CarbonateHCID 13677741Ethyl cis-3-methoxy-4-[(phenylmethyl)amino]-1-piperidinecarboxylate

생성물 1

HCID 67922776HCID 67922776, 화합물수율 64%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 183.4 parts of ethyl cis-3-methoxy-4-[(phenylmethyl)amino]-1-piperidinecarboxylate, 144 parts of (chloromethyl)benzene, 85 parts of sodium carbonate and 720 parts of methylbenzene was stirred for 10 days at reflux temperature. The reaction mixture was filtered and the filtrate was washed three times with 400 parts of water, dried, filtered and evaporated. Petroleumether was added. The whole was cooled whereupon the product solidified. It was filtered off and crystallized from petroleumether. The product was filtered off and dried in vacuo at 40° C., yielding 155 parts (64%) of ethyl cis-4-[bis(phenylmethyl)amino]-3-methoxy-1-piperidinecarboxylate; mp. 95.2° C. (int. 46).

후처리

  1. temperatureat reflux temperature
  2. filtrationThe reaction mixture was filtered
  3. washthe filtrate was washed three times with 400 parts of water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. additionPetroleumether was added
  8. temperatureThe whole was cooled whereupon the product
  9. filtrationIt was filtered off
  10. customcrystallized from petroleumether
  11. filtrationThe product was filtered off
  12. customdried in vacuo at 40° C.

출처 및 근거

ORD 기록
ord-bf36a41cb21845ccb52c1be4071f431b
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04975439

반응 노트

불러오는 중…