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Ammonium Chloride → HCID 86646304, 화합물

HRID 1027136
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HRID 1027136 반응식
[CH3:1][C:2]1(O)[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:4]2([CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]2)[CH2:3]1.O.C1(C)C(S(O)(=O)=O)=CC=CC=1.[Cl-].[NH4+]>C(Cl)Cl>[CH3:1][C:2]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:4]2([CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:14])([CH3:15])[CH3:16])=[O:11])[CH2:6][CH2:5]2)[CH:3]=1
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참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 124969952-Methylbenzenesulfonic acid hydrateHCID 67082928tert-Butyl 1-methyl-1-hydroxyspiro[indane-3,4'-piperidine]-1'-carboxylate

생성물 1

HCID 86646304HCID 86646304, 화합물수율 81.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

tert-Butyl 1-methyl-1-hydroxyspiro[indane-3,4′-piperidine]-1′-carboxylate (0.140 g, 0.441 mmol) obtained in step 1 was dissolved in methylene chloride (2 mL), toluenesulfonic acid monohydrate (0.008 g, 0.044 mmol) was added, and the mixture was stirred at room temperature for 3 hr. Saturated aqueous ammonium chloride solution was added dropwise to the reaction mixture, and the mixture was extracted several times with ethyl acetate. The combined organic layers were dried over magnesium sulfate and concentrated under reduced pressure to give the title compound (0.108 g, 81%).

후처리

  1. extractionthe mixture was extracted several times with ethyl acetate
  2. dry with materialThe combined organic layers were dried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2b84a62b41144231829142f49ac6e675
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729264B2

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