Acetyl chloride → 3-Acetoxycyclobutanecarboxylic acid

HRID 520708노트

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HRID 520708 반응식
[OH:1][CH:2]1[CH2:5][CH:4]([C:6]([OH:8])=[O:7])[CH2:3]1.[C:9](Cl)(=[O:11])[CH3:10]>C(Cl)Cl.CN(C1C=CN=CC=1)C>[C:9]([O:1][CH:2]1[CH2:5][CH:4]([C:6]([OH:8])=[O:7])[CH2:3]1)(=[O:11])[CH3:10]

참가 물질

5

반응물 2

HCID 6367Acetyl chlorideHCID 226409863-Hydroxycyclobutane-1-carboxylic acid

생성물 1

HCID 898403503-Acetoxycyclobutanecarboxylic acid

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

To a solution of 3-hydroxycyclobutanecarboxylic acid (100 mg, 0.86 mmol) in DCM (10 mL) was added DMAP (1.0 mg, 0.086 mmol). The solution was cooled to 0° C., followed by the addition of acetyl chloride (0.14 mL, 2.6 mmol). The reaction was heated at 45° C. for 4 hours, then cooled to rt and diluted with DCM (20 mL). The mixture was washed with water (10 mL), followed by washing with brine (10 mL), dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to obtained the crude product which was used in the next step without further purification.

후처리

  1. temperatureThe reaction was heated at 45° C. for 4 hours
  2. temperaturecooled to rt
  3. washThe mixture was washed with water (10 mL)
  4. washby washing with brine (10 mL)
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b79975aeeaa84de298d65b5fda134ede
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09326975B2

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