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Sodium Hydroxide → 3-Benzyl-1,2,4-oxadiazol-5(2H)-one

HRID 1076951
ノート
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反応式

HRID 1076951 の反応式
[C:1]1([CH2:7][C:8]2[N:12]=[C:11](C(Cl)(Cl)Cl)[O:10][N:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-:17].[Na+]>C(O)C>[C:1]1([CH2:7][C:8]2[NH:12][C:11](=[O:17])[O:10][N:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 215332303-(Phenylmethyl)-5-trichloromethyl-1,2,4-oxadiazole

生成物 1

HCID 1356776173-Benzyl-1,2,4-oxadiazol-5(2H)-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

60 g. (0.22 moles) of 3-(phenylmethyl)-5-trichloromethyl-1,2,4-oxadiazole is dissolved in 100 ml. of ethanol. The solution is stirred and 132 ml. (0.264 mole) of 2N sodium hydroxide solution are added dropwise. The temperature of the mixture rises to about 40°. After the addition has been completed, the mixture is stirred for an additional 30 minutes and then concentrated in a rotary evaporator. The residue is treated with water, filtered and the filtrate is acidified with 2N hydrochloric acid. The crystals are filtered under suction, and purified by dissolving in sodium bicarbonate solution, filtering and precipitating with dilute hydrochloric acid. 29.7 g. of 3-(phenylmethyl)-1,2,4-oxadiazol-5-(4H)-one are obtained, m.p. 114°-116°.

後処理

  1. customrises to about 40°
  2. additionAfter the addition
  3. stirringthe mixture is stirred for an additional 30 minutes
  4. concentrationconcentrated in a rotary evaporator
  5. additionThe residue is treated with water
  6. filtrationfiltered
  7. filtrationThe crystals are filtered under suction
  8. custompurified
  9. dissolutionby dissolving in sodium bicarbonate solution
  10. filtrationfiltering
  11. customprecipitating with dilute hydrochloric acid

出典と根拠

ORDレコード
ord-827aa8783cc4491787e14643fc4b5419
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03959259

反応ノート

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