Chloroform → HCID 13314616, 화합물

HRID 543575

반응식

HRID 543575 반응식
Cl.[O:2]1[CH2:6][CH2:5][CH2:4][NH:3]1.C(Cl)(Cl)Cl.[Cl:11][CH:12]([CH3:16])[C:13](Cl)=[O:14].C(N(CC)CC)C>O>[Cl:11][CH:12]([CH3:16])[C:13]([N:3]1[CH2:4][CH2:5][CH2:6][O:2]1)=[O:14]

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 8471TriethylamineHCID 1110192-Chloropropionyl chlorideHCID 12304500Isoxazolidine hydrochloride

생성물 1

HCID 13314616HCID 13314616, 화합물수율 91.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of isoxazolidine hydrochloride (11.0 g) and chloroform (200 ml) was added (±)-2-chloropropionyl chloride (13.3 g) under ice-cooling and stirring and then added dropwise triethylamine (22.2 g) under the same conditions. The stirring was continued at room temperature for further one hour, after which an amount of water was added to the reaction mixture to form layers. The organic layer thus separated was washed with 1 N hydrochloric acid and then with a 5% aqueous sodium bicarbonate solution and dried over anhydrous sodium sulfate. Removal of the solvent by a distillation in vacuo gave N-[(±)-2-chloropropionyl]isoxazolidine (15.0 g) as a pale yellow oil. Purification of the oil by silica gel column chromatography afforded a colorless oil. nD20 =1.4918.

후처리

  1. temperaturecooling
  2. customto form layers
  3. customThe organic layer thus separated
  4. washwas washed with 1 N hydrochloric acid
  5. dry with materialwith a 5% aqueous sodium bicarbonate solution and dried over anhydrous sodium sulfate
  6. customRemoval of the solvent
  7. distillationby a distillation in vacuo

출처 및 근거

ORD 기록
ord-a2395f5bbfa940c9a5a470319191bb8c
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04447259

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