Hydrochloric Acid → 5-(4-phenoxyphenyl)-7-(4-piperidyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine dihydrochloride

HRID 51525

반응식

HRID 51525 반응식
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:22]3[C:21]([NH2:23])=[N:20][CH:19]=[N:18][C:17]=3[N:16]([CH:24]3[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]3)[CH:15]=2)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCOCC.[ClH:35]>CCOC(C)=O.CO>[ClH:35].[ClH:35].[O:1]([C:8]1[CH:9]=[CH:10][C:11]([C:14]2[C:22]3[C:21]([NH2:23])=[N:20][CH:19]=[N:18][C:17]=3[N:16]([CH:24]3[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]3)[CH:15]=2)=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 101615435-(4-phenoxyphenyl)-7-(4-piperidyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine

생성물 1

HCID 101615425-(4-phenoxyphenyl)-7-(4-piperidyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine dihydrochloride

시약·촉매·용매 1

HCID 21584119Ethylacetate methanol용매

실험 절차

To 5-(4-phenoxyphenyl)-7-(4-piperidyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine (433258) (200 mg) in EtOAc/MeOH (15 ml, 1:1) was added ether.HCl solution (1.0 M, 3 ml). The resulting white precipitate was filtered under a stream of nitrogen and dried in vacuo for 6 hr to leave 5-(4-phenoxyphenyl)-7-(4-piperidyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine dihydrochloride (1.4 hydrate) as a white solid (120 mg), m.pt. 304° C (dec.). 1H NMR (D2O, 250 MHz) 8.48(1H, s), 7.69 (1H, s), 7.50-7.58 (4H, m), 7.18-7.34 (5H, m), 5.16 (1H, m), 3.81 (2H, d), 3.46 (2H, m), 2.49 (4H, m).). IR (KBr disc): 3937, 1657, 1231 cm−1.

후처리

  1. filtrationThe resulting white precipitate was filtered under a stream of nitrogen
  2. customdried in vacuo for 6 hr

출처 및 근거

ORD 기록
ord-e7c0e80967f649469365b814341842cc
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06713474B2

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