Diethyl Ether → HCID 13631104、化合物

HRID 2413709ノート

反応式

HRID 2413709 の反応式
[O:1]=[C:2]1[CH2:5][CH2:4][N:3]1[CH2:6][C:7]([O:9]CC)=O.O.[NH3:13].C(Cl)(Cl)Cl.CCOCC>CO>[O:1]=[C:2]1[CH2:5][CH2:4][N:3]1[CH2:6][C:7]([NH2:13])=[O:9]

参加物

6

実験手順

In 0.8 ml of methanol was dissolved 843 mg of compound (19) and 0.4 ml of conc. ammonia water was added to the solution under ice cooling followed by stirring at room temperature for 18 hours. The reaction mixture was concentrated under reduced pressure. The residue was purified by column chromatography (30 g of silica gel, chloroform-methanol=10:1) to obtain 550 mg of a roughly purified product. The product was treated with a solvent mixture of 3 ml of chloroform and 3 ml of ether to crystallize. Thus 360 mg of α-(2-oxo-1-azetidinyl)acetamide (22) was obtained as colorless crystals.

後処理

  1. additionwas added to the solution under ice cooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customThe residue was purified by column chromatography (30 g of silica gel, chloroform-methanol=10:1)
  4. customto obtain 550 mg of a roughly purified product
  5. customto crystallize

出典と根拠

ORDレコード
ord-58eab94efa0847459be40573bd5bc63d
出典データセット
uspto-grants-1988_01
特許番号
US04719207

反応ノート

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