Sulfuric Acid → HCID 15147196, 화합물

HRID 380494노트

반응식

HRID 380494 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][O:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O.OS(O)(=O)=O>O>[F:23][C:20]1[CH:19]=[CH:18][C:17]([CH2:16][O:15][CH2:14][CH:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[CH:22][CH:21]=1

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 6422Trifluoroacetic acidHCID 183647941-t-Butoxycarbonyl-4-(4-fluorobenzyloxymethyl)piperidine

생성물 1

HCID 15147196HCID 15147196, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 0.89 g (2.35 mmol) of 1-t-butoxycarbonyl-4-(4-fluorobenzyloxymethyl)piperidine in 8 mL of H2O at rt was added 2 mL of TFA and the reaction mixture was stirred for 2 h. To the reaction mixture was added 50 mL of 0.5N H2SO4. After stirring vigorously for 5 min, the mixture was was washed with CH2Cl2. The aqueous fraction was made basic with solid K2CO3 and extracted with CH2Cl2. The combined organic fractions were washed with sat'd NaCl solution, dried over MgSO4 and filtered. The filtrate was concentrated to give the title compound.

후처리

  1. stirringAfter stirring vigorously for 5 min
  2. washthe mixture was was washed with CH2Cl2
  3. extractionextracted with CH2Cl2
  4. washThe combined organic fractions were washed with sat'd NaCl solution
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-d451e90670114232bde467b089f4d0e0
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06303593B1

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