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

HRID 2261309

反応式

HRID 2261309 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bb856fa08426417186d5bd3dcc06cc15
出典データセット
uspto-grants-2010_12
特許番号
US07846956B2

関連ノート

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