Hydrochloric Acid → Ethyl 3-fluoro-4-cyclohexylphenylglyoxylate

HRID 426794

反応式

HRID 426794 の反応式
N[C:2]1[CH:3]=[C:4]([C:14](=[O:20])[C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH:5]=[CH:6][C:7]=1[CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.Cl.[N+]([O-])([O-])=O.[Na+].B(O)(O)O.[FH:31]>O>[F:31][C:2]1[CH:3]=[C:4]([C:14](=[O:20])[C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH:5]=[CH:6][C:7]=1[CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 7628Boric AcidHCID 14917Hydrofluoric AcidHCID 24268Sodium NitrateHCID 20515218Ethyl 3-amino-4-cyclohexylphenylglyoxylate

生成物 1

HCID 20515163Ethyl 3-fluoro-4-cyclohexylphenylglyoxylate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

To 44.2 g. (0.15 moles) of ethyl 3-amino-4-cyclohexylphenylglyoxylate is added at 0° C. 44 ml. of 1.5 moles of concentrated hydrochloric acid. The reaction is maintained at 0° C. and the diazonium salt is prepared with 23.2 g. (0.32 moles) of 95% sodium nitrate in 80 ml. of water. To this mixture is rapidly added a solution of 10.4 g. (0.17 moles) of boric acid dissolved in 22 g. (0.66 moles) of 60% hydrofluoric acid. The reaction mixture is then stirred for 1/2 hour and filtered, washed with 3×25 ml. of water, 2×25 ml. of methanol and 25 ml. of ether. The residual cake is then treated in vacuo. The treated cake is then placed in a distilling flask and heated to permit spontaneous decomposition. After the decomposition, the residue is then fractionally distilled to obtain ethyl 3-fluoro-4-cyclohexylphenylglyoxylate.

後処理

  1. additionTo this mixture is rapidly added a solution of 10.4 g
  2. filtrationfiltered
  3. washwashed with 3×25 ml
  4. additionThe residual cake is then treated in vacuo
  5. customThe treated cake is then placed in a distilling flask
  6. temperatureheated
  7. distillationAfter the decomposition, the residue is then fractionally distilled

出典と根拠

ORDレコード
ord-aaf8046a80194a5dbd56923dc7c2416e
出典データセット
uspto-grants-1979_10
特許番号
US04171373

関連ノート

読み込み中…