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Trimethyl orthobeznoate → HCID 20323691、化合物

HRID 839581
ノート
印刷プレビュー

反応式

HRID 839581 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]([NH:8][NH2:9])=[O:7].CO[C:12](OC)(OC)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(O)C>[C:13]1([C:12]2[N:1]3[CH:5]=[CH:4][N:3]=[C:2]3[C:6](=[O:7])[NH:8][N:9]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=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 69720Trimethyl orthobeznoateHCID 12493320HCID 12493320、化合物

生成物 1

HCID 20323691HCID 20323691、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A 2.6 gm. portion of 2-imidazolecarboxylic acid hydrazide is added to 200 ml. of ethanol. To this is added 20 ml. of trimethylorthobenzoate. The mixture is refluxed for 31 hours, then the solvents are evaporated giving a white solid which is washed twice with diethyl ether giving 3.0 gm. of white solid. This solid is combined with 50 ml. of diphenyl ether and heated with stirring in an oil bath at 265°-275° C. for 10 minutes. The mixture is cooled, petroleum ether is added and the mixture is filtered. The solid is washed twice with hot petroleum ether, giving 1.4 gm. of the desired product as a light tan solid, m.p. 292°-295° C.

後処理

  1. additionTo this is added 20 ml
  2. temperatureThe mixture is refluxed for 31 hours
  3. customthe solvents are evaporated
  4. customgiving a white solid which
  5. washis washed twice with diethyl ether giving 3.0 gm
  6. temperatureof diphenyl ether and heated
  7. temperatureThe mixture is cooled
  8. additionpetroleum ether is added
  9. filtrationthe mixture is filtered
  10. washThe solid is washed twice with hot petroleum ether
  11. customgiving 1.4 gm

出典と根拠

ORDレコード
ord-f8ec96467a4c423aad6f340a91e45337
出典データセット
uspto-grants-1978_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04096257

反応ノート

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