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Sodium triacetoxyborohydride → HCID 86633670, 화합물

HRID 1642028
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HRID 1642028 반응식
[F:1][C:2]([F:30])([F:29])[O:3][C:4]1[CH:9]=[CH:8][C:7]([CH:10]([C:18]2[CH:23]=[CH:22][C:21]([O:24][C:25]([F:28])([F:27])[F:26])=[CH:20][CH:19]=2)[C:11]2([OH:17])[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:6][CH:5]=1.[CH3:31][O:32][CH2:33][CH2:34][O:35][C:36]1[CH:43]=[CH:42][C:39]([CH:40]=O)=[CH:38][CH:37]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(Cl)Cl.O>[F:27][C:25]([F:28])([F:26])[O:24][C:21]1[CH:22]=[CH:23][C:18]([CH:10]([C:7]2[CH:6]=[CH:5][C:4]([O:3][C:2]([F:29])([F:1])[F:30])=[CH:9][CH:8]=2)[C:11]2([OH:17])[CH2:16][CH2:15][N:14]([CH2:40][C:39]3[CH:38]=[CH:37][C:36]([O:35][CH2:34][CH2:33][O:32][CH3:31])=[CH:43][CH:42]=3)[CH2:13][CH2:12]2)=[CH:19][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 5049666Sodium triacetoxyborohydrideHCID 64855604-(2-Methoxyethoxy)benzaldehydeHCID 166562744-{Bis[4-(trifluoromethoxy)phenyl]methyl}piperidin-4-ol

생성물 1

HCID 86633670HCID 86633670, 화합물수율 73.4%

시약·촉매·용매 2

HCID 962Water용매
HCID 6344
Dichloromethane
용매

실험 절차

A solution of 2.2 grams (0.0050 mole) of 4-{bis[4-(trifluoromethoxy)phenyl]methyl}piperidin-4-ol, 1.1 grams (0.0061 mole) of 4-(2-methoxyethoxy)benzaldehyde and 1.35 grams (0.0064 mole) of sodium triacetoxyborohydride in 25 mL of methylene chloride was stirred at ambient temperature for 18 hours. The reaction mixture was then diluted with 200 mL of water and stirred at ambient temperature for 5 hours. The phases were separated. The organic phase was washed three times; first, with 100 mL of an aqueous mixture of 10% sodium hydroxide, second, with 100 mL of an aqueous mixture of 10% lithium chloride, and, third, with 100 mL of brine. The resultant organic layer was dried over magnesium sulfate, filtered and concentrated under reduced pressure to a residue. The residue was purified with column chromatography on silica gel using methylene chloride:1%-5% methanol as an eluant. The appropriate fractions were combined and concentrated under reduced pressure, yielding 2.2 grams of the subject compound. The NMR spectrum was consistent with the proposed structure.

후처리

  1. customThe phases were separated
  2. washThe organic phase was washed three times
  3. dry with materialThe resultant organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure to a residue
  6. customThe residue was purified with column chromatography on silica gel
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b71c28e5306043eb965408b4d722722f
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08119563B2

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