Hydrochloric Acid → HCID 19426302, 화합물

HRID 2210295노트

반응식

HRID 2210295 반응식
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][CH:12]([OH:15])[CH:11]([N:16]2[CH2:21][CH2:20][C:19]3([C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[CH2:24][CH2:23][CH2:22]3)[CH2:18][CH2:17]2)[CH2:10]1)=O)(C)(C)C>CCOC(C)=O>[ClH:1].[ClH:1].[OH:15][CH:12]1[CH2:13][CH2:14][NH:9][CH2:10][CH:11]1[N:16]1[CH2:21][CH2:20][C:19]2([C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:24][CH2:23][CH2:22]2)[CH2:18][CH2:17]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 104536361'-(1-t-butoxycarbonyl-4-hydroxypiperidin-3-yl)-3,4-dihydro-spiro[naphthalene-1(2H),4'-piperidine]

생성물 1

HCID 19426302HCID 19426302, 화합물수율 80%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

HCl gas was bubbled for 30 min through a soln of 20c (800 mg, 2.1 mmol) in EtOAc (10 mL) while the flask was maintained in an ice bath. The resulting solution was subsequently stirred at room temperature for 30 min, and the volatiles were removed under reduced pressure. The white solid thus obtained was recrystallized from 50% isopropyl alcohol-hexanes to provide the hydrochlorides of 21c as a white powder (80%). Elemental analysis: Calc: C=61.12, H=8.1, N=7.5; Fnd: C=59.96, H=Elemental analysis: Gale: C=61.12, H=8.1, N=7.5; Fnd: C=59.96, H=7.95, N=6.86.

후처리

  1. temperaturewas maintained in an ice bath
  2. customthe volatiles were removed under reduced pressure
  3. customThe white solid thus obtained
  4. customwas recrystallized from 50% isopropyl alcohol-hexanes

출처 및 근거

ORD 기록
ord-dfe0ae88f8fe456eb7515451ac263bca
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05457207

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