Sodium Bicarbonate → 2-Tert-butyl-5-(chloromethyl)-1,3,4-oxadiazole

HRID 2261309

반응식

HRID 2261309 반응식
[Cl:1][CH2:2][C:3]([NH:5][NH:6][C:7](=[O:12])[C:8]([CH3:11])([CH3:10])[CH3:9])=O.C(=O)(O)[O-].[Na+]>O>[C:8]([C:7]1[O:12][C:3]([CH2:2][Cl:1])=[N:5][N:6]=1)([CH3:9])([CH3:10])[CH3:11]

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 54595759N'-(2-chloroacetyl)-2,2-dimethylpropanehydrazide

생성물 1

HCID 167787622-Tert-butyl-5-(chloromethyl)-1,3,4-oxadiazole수율 92.2%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

A mixture of 1.34 g of N′-(chloroacetyl)-2,2-dimethylpropanohydrazide and 6.6 g of polyphosphoric acid was stirred at 90° C. for 10 hours. The reaction mixture was cooled to room temperature. After 200 ml of water and then sodium bicarbonate were added, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous sodium sulfate and then concentrated under reduced pressure to obtain 1.12 g of 2-t-butyl-5-(chloromethyl)-1,3,4-oxadiazole.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-bb856fa08426417186d5bd3dcc06cc15
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07846956B2

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