Acetyl chloride → 3-Acetoxycyclobutanecarboxylic acid

HRID 520708ノート

反応式

HRID 520708 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 898403503-Acetoxycyclobutanecarboxylic acid

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b79975aeeaa84de298d65b5fda134ede
出典データセット
uspto-grants-2016_05
特許番号
US09326975B2

反応ノート

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