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Hydrochloric Acid → HCID 178479255, 화합물

HRID 2265902
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HRID 2265902 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[C:26]4[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=4[O:24][N:23]=3)[CH2:18][CH2:17]2)[CH2:10][CH2:9]1)(C)(C)C.[ClH:32].O1CCOCC1>ClCCl.C(OC(C)C)(C)C>[ClH:32].[O:24]1[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[C:22]([N:19]2[CH2:18][CH2:17][N:16]([CH2:15][CH2:14][C@H:11]3[CH2:12][CH2:13][C@H:8]([NH2:7])[CH2:9][CH2:10]3)[CH2:21][CH2:20]2)=[N:23]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 178453913HCID 178453913, 화합물

생성물 1

HCID 178479255HCID 178479255, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 7914Diisopropyl Ether용매

실험 절차

Trans-{4-[2-(4-Benzo[d]isoxazol-3-yl-piperazin-1-yl)-ethyl]-cyclohexyl}-carbamic acid tert-butyl ester (1.3 g, 3.03 mmol) was dissolved in 3 ml dichloromethane and 4N HCl in dioxane (15.2 ml, 60.7 mmol) was added. The white suspension was stirred for 4 hours at room temperature, diluted with diisopropylether and filtered. The crystals were washed with diisopropylether and dried for 1 hour at 50° C. and <20 mbar, to get the desired salt as a white solid (1.2 g, quant.) [MS: m/e=329.2 (M+H+)].

후처리

  1. filtrationfiltered
  2. washThe crystals were washed with diisopropylether
  3. customdried for 1 hour at 50° C.

출처 및 근거

ORD 기록
ord-f9ea43ce931b4937aba2b8f837e0c199
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858630B2

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