Acetic Anhydride → 1,3-Dipivaloyl-2-acetoxymethyl glycerol

HRID 483675노트

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HRID 483675 반응식
[C:1]([O:7][CH2:8][CH:9]([CH2:14][O:15][C:16](=[O:21])[C:17]([CH3:20])([CH3:19])[CH3:18])OCOC)(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].[C:22]([O:25][C:26](=[O:28])[CH3:27])(=[O:24])C.B(F)(F)F.CCOCC>C(Cl)Cl>[C:1]([O:7][CH2:8][CH:9]([CH2:14][O:15][C:16](=[O:21])[C:17]([CH3:20])([CH3:19])[CH3:18])[O:24][CH2:22][O:25][C:26](=[O:28])[CH3:27])(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8000Boron trifluoride etherateHCID 109796251,3-Dipivaloyl-2-methoxymethyl glycerol

생성물 1

HCID 110458291,3-Dipivaloyl-2-acetoxymethyl glycerol

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

50 g of 1,3-dipivaloyl-2-methoxymethyl glycerol, 150 ml of methylene chloride, and 17 ml of acetic anhydride was cooled to about -5° C. Then 0.3 ml of boron trifluoride etherate was added and the mixture was stirred for an additional 1 hr at about 0° C. then allowed to warm to 25° C. over an additional 1.5 hr. After this period, 100 ml saturated aqueous Na2Cl3 was added to the mixture followed by 100 ml CH2Cl2. After vigorous stirring for 5 min, the organic layer was separated and washed once with 100 ml H2O, once with aqueous NaCl, dried over anhydrous magnesium sulfate and concentrated in vacuo to afford 1,3-dipivaloyl-2-acetoxymethyl glycerol as a faintly colored oil.

후처리

  1. temperatureto warm to 25° C. over an additional 1.5 hr
  2. waitAfter this period
  3. stirringAfter vigorous stirring for 5 min
  4. customthe organic layer was separated
  5. washwashed once with 100 ml H2O, once with aqueous NaCl
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-dbeb750e3a844d4aaa2776fe2a154fb8
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05225590

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