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Hydrochloric Acid → HCID 178478590, 화합물

HRID 1260705
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HRID 1260705 반응식
C(OC(=O)[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][N:19]([C:22]3[N:23]=[CH:24][CH:25]=[C:26]4[CH2:30][CH2:29][O:28][C:27]=34)[CH2:18][CH2:17]2)[CH2:10][CH2:9]1)(C)(C)C.[ClH:32]>ClCCl>[ClH:32].[ClH:32].[ClH:32].[O:28]1[C:27]2=[C:22]([N:19]3[CH2:20][CH2:21][N:16]([CH2:15][CH2:14][C@H:11]4[CH2:12][CH2:13][C@H:8]([NH2:7])[CH2:9][CH2:10]4)[CH2:17][CH2:18]3)[N:23]=[CH:24][CH:25]=[C:26]2[CH2:30][CH2:29]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178453909HCID 178453909, 화합물

생성물 1

HCID 178478590HCID 178478590, 화합물수율 97.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of trans-(4-{2-[4-(2,3-dihydro-furo[2,3-c]pyridin-7-yl)-piperazin-1-yl]-ethyl}-cyclohexyl)-carbamic acid tert-butyl ester (1.3 g, 3.02 mmol) in dichloromethane (21 ml) was added at room temperature hydrochloric acid solution (4M in dioxane, 11.3 ml, 45.3 mmol) and the mixture was allowed to stir for 3 h, the solvent was evaporated, diethyl ether (50 ml) was added and the mixture was allowed to stir for 30 min at room temperature. The precipitate was collected by filtration, washed with diethyl ether and dried to yield the title compound as off-white solid (1.29 g, 97%), MS (ISP) m/z=331.3 [(M+H)+], mp 318.5° C.

후처리

  1. customthe solvent was evaporated
  2. additiondiethyl ether (50 ml) was added
  3. stirringto stir for 30 min at room temperature
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with diethyl ether
  6. customdried

출처 및 근거

ORD 기록
ord-953439edcc294d6fa346b52698782e07
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08470828B2

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