Ammonia → HCID 19785352, 화합물

HRID 2248803노트

반응식

HRID 2248803 반응식
[C:1]1([CH2:7][NH:8][C:9]2[C:14]([NH:15][C:16]([NH:18][CH:19]3[CH2:24][CH2:23][N:22]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH2:21][CH2:20]3)=S)=[CH:13][N:12]=[CH:11][N:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N>[Hg]=O.CO>[C:1]1([CH2:7][N:8]2[C:16]([NH:18][CH:19]3[CH2:24][CH2:23][N:22]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH2:21][CH2:20]3)=[N:15][C:14]3[C:9]2=[N:10][CH:11]=[N:12][CH:13]=3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 19785231HCID 19785231, 화합물

생성물 1

HCID 19785352HCID 19785352, 화합물수율 92.1%

시약·촉매·용매 2

HCID 30856Mercuric oxide촉매HCID 887Methanol용매

실험 절차

A mixture of 24 parts of ethyl 4-[[[[4-[(phenylmethyl)amino]-5-pyrimidinyl]amino]thioxomethyl]amino]-1-piperidinecarboxylate, 24 parts of mercury(II) oxide and 240 parts of methanol, saturated with ammonia was stirred overnight at reflux temperature. The reaction mixture was filtered while hot and the filtrate was evaporated. The residue was taken up in a mixture of trichloromethane and ethanol. After washing with water, the organic layer was evaporated and the residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 20.3 parts (92.1%) of ethyl 4-[[9-(phenylmethyl)-9H-purin-8-yl]amino]-1-piperidinecarboxylate; mp. 156.9° C. (compound 9).

후처리

  1. temperatureat reflux temperature
  2. filtrationThe reaction mixture was filtered while hot and the filtrate
  3. customwas evaporated
  4. additionThe residue was taken up in a mixture of trichloromethane and ethanol
  5. washAfter washing with water
  6. customthe organic layer was evaporated
  7. customthe residue was crystallized from acetonitrile
  8. filtrationThe product was filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-97cc647595e5402985b2704b4fb500fc
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05041448

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