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Sulfuric Acid → HCID 23149943, 화합물

HRID 238272
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HRID 238272 반응식
C(OC([N:8]1[CH2:13][CH2:12][C:11]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][C:16]=2[F:22])(O)[CH2:10][CH2:9]1)=O)(C)(C)C.S(=O)(=O)(O)O.[OH-].[Na+]>C1(C)C=CC=CC=1>[F:22][C:16]1[CH:17]=[C:18]([F:21])[CH:19]=[CH:20][C:15]=1[C:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 497602291-Boc-4-(2,4-difluorophenyl)-4-hydroxypiperidine

생성물 1

HCID 23149943HCID 23149943, 화합물수율 80.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

4-(2,4-Difluoro-phenyl)-4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (0.4 g) was dissolved in toluene (10 mL). Concentrated sulphuric acid (0.3 mL) was added and the mixture was heated at reflux for 2 hours and then allowed to stand at room temperature overnight. A solution of aqueous sodium hydroxide (1 N, 30 mL) was added and the products extracted into ethyl acetate. The organic solution was dried with magnesium sulphate, filtered and the solvent removed by evaporation under vacuum to give the title compound as a dark oil (0.2 g) which was used without further purification. LCMS m/z 196.1 [M+H]+. R.T.=2.12 min (Analytical Method 4).

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. extractionthe products extracted into ethyl acetate
  4. dry with materialThe organic solution was dried with magnesium sulphate
  5. filtrationfiltered
  6. customthe solvent removed by evaporation under vacuum

출처 및 근거

ORD 기록
ord-a12ae00f53b8499dbc78f8a8d8154f3d
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08642621B2

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