Sulfuric Acid → HCID 15147196、化合物

HRID 380494ノート

反応式

HRID 380494 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 15147196HCID 15147196、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d451e90670114232bde467b089f4d0e0
出典データセット
uspto-grants-2001_10
特許番号
US06303593B1

反応ノート

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