Benzyl Chloride → HCID 67922776、化合物

HRID 2248624ノート

反応式

HRID 2248624 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 67922776HCID 67922776、化合物収率 64%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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.

出典と根拠

ORDレコード
ord-0bf50e6208ac4d5c9b785fb9203176f5
出典データセット
uspto-grants-1991_08
特許番号
US05041454

反応ノート

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