Pentadecalactone → 15-Bromopentadecanoic acid

HRID 2061919

반응식

HRID 2061919 반응식
[C:1]1(=[O:17])[O:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[BrH:18].C(O)(=O)C>>[Br:18][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][C:1]([OH:16])=[O:17]

참가 물질

3

반응물 2

HCID 235414PentadecalactoneHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

생성물 1

HCID 55229615-Bromopentadecanoic acid

실험 절차

15-Pentadecanolide of 14.3 g (59.5 mmol), and 32% hydrogen bromide/acetic acid solution of 24.8 g (98.0 mmol, 1.6 eq) were added to 100 mL of autoclave protected with Teflon (registered trade name). After purging with nitrogen and sealing, the autoclave was placed in an oil bath at 60° C. and stirring was carried out for 16 hours. For the stirring, a magnetic stirrer was used. After cooling, 14 mL of water was added, and by using 200 mL of hot hexane the mixture was transferred to a separatory funnel. After washing with ion exchange water, it was dried over the magnesium sulfate. After filtration, 17.4 g of the target compound was obtained by crystallization using n-hexane (yield 91%).

후처리

  1. customAfter purging with nitrogen and sealing
  2. customthe autoclave was placed in an oil bath at 60° C.
  3. temperatureAfter cooling
  4. addition14 mL of water was added
  5. customwas transferred to a separatory funnel
  6. washAfter washing with ion exchange water, it
  7. dry with materialwas dried over the magnesium sulfate
  8. filtrationAfter filtration

출처 및 근거

ORD 기록
ord-174a689a009a49f29000d85f1040ca4b
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08283482B2

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