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Hydrochloric Acid → 7,9-Difluoro-5-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-5H-6-oxa-chrysen-2-ol hydrochloride salt

HRID 1513923
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HRID 1513923 반응식
[F:1][C:2]1[CH:19]=[C:18]([F:20])[CH:17]=[C:16]2[C:3]=1[O:4][CH:5]([C:22]1[CH:27]=[CH:26][C:25]([O:28][CH2:29][CH2:30][N:31]3[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]3)=[CH:24][CH:23]=1)[C:6]1[C:15]2=[CH:14][CH:13]=[C:12]2[C:7]=1[CH:8]=[CH:9][C:10]([OH:21])=[CH:11]2.[ClH:37].CCOCC>C(Cl)Cl>[ClH:37].[F:1][C:2]1[CH:19]=[C:18]([F:20])[CH:17]=[C:16]2[C:3]=1[O:4][CH:5]([C:22]1[CH:23]=[CH:24][C:25]([O:28][CH2:29][CH2:30][N:31]3[CH2:32][CH2:33][CH2:34][CH2:35][CH2:36]3)=[CH:26][CH:27]=1)[C:6]1[C:15]2=[CH:14][CH:13]=[C:12]2[C:7]=1[CH:8]=[CH:9][C:10]([OH:21])=[CH:11]2
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 117850637,9-Difluoro-5-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-5H-6-oxa-chrysen-2-ol

생성물 1

HCID 670045857,9-Difluoro-5-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-5H-6-oxa-chrysen-2-ol hydrochloride salt수율 87%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Dissolve 7,9-difluoro-5-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-5H-6-oxa-chrysen-2-ol (1.6 g, 3.3 mmol) in methylene chloride (20 mL). Add 2M HCl in ether (3.3 mL, 6.6 mmol) and concentrate in vacuo. Dissolve the residue in methylene chloride (5 mL) and add dropwise to vigorously stirred ether (30 mL). Filter the precipitate and dry in a 50° C. vacuum oven overnight to obtain 1.5 g (87%) of the title compound. Mass spectrum (ion spray): m/z=488.3 (M+H−HCl).

후처리

  1. concentrationconcentrate in vacuo
  2. dissolutionDissolve the residue in methylene chloride (5 mL)
  3. additionadd dropwise to vigorously stirred ether (30 mL)
  4. filtrationFilter the precipitate
  5. customdry in a 50° C. vacuum oven overnight

출처 및 근거

ORD 기록
ord-db292954e3604b609c6075153bf71c04
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08217032B2

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