Chloroacetyl chloride → HCID 15174914、化合物

HRID 359067

反応式

HRID 359067 の反応式
Cl.[O:2]1[CH2:6][CH2:5][CH2:4][NH:3]1.C(N(CC)CC)C.[Cl:14][CH2:15][C:16](Cl)=[O:17]>CCOCC>[Cl:14][CH2:15][C:16]([N:3]1[CH2:4][CH2:5][CH2:6][O:2]1)=[O:17]

参加物

5

実験手順

To a stirred slurry of finely powdered isooxazolidine hydrochloride (H. King, J. Chem. Soc. 433,1942) (11.0 g) in dry ether (200 ml) at 0° C. was added triethylamine (28.0 ml) and a solution of chloroacetyl chloride (8.0 ml) in ether (50 ml). The reaction mixture was stirred for a further 4 hours, whilst the temperature rose to room temperature. The precipitate triethylamine hydrochloride was filtered off through diatomaceous earth and the filter bed washed well with ether. The combined ether solutions were evaporated to give N-chloroacetyl isooxazolidine as an oil (11.5 g) NMR (CDCl3) 2.38[quintet, 2H, CH2 ], 3.78[t,2H, NCH2 ], 4.05[t,2H, OCH2 ]and 4.22 [s,2H, ClCH2CO].

後処理

  1. customrose to room temperature
  2. filtrationThe precipitate triethylamine hydrochloride was filtered off through diatomaceous earth
  3. washthe filter bed washed well with ether
  4. customThe combined ether solutions were evaporated

出典と根拠

ORDレコード
ord-058e5c4a27c645e7becd71851b9369ff
出典データセット
uspto-grants-1991_03
特許番号
US04999377

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