Hydrochloric Acid → HCID 22760937、化合物

HRID 1605636ノート

反応式

HRID 1605636 の反応式
O=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[CH2:3]1.[O-]CC.[Na+].[CH3:21][C:22]([CH:24]=[CH2:25])=[O:23].Cl>C(O)C>[O:23]=[C:22]1[CH2:24][CH2:25][C:3]2[C:4]3[CH:16]=[CH:15][CH:14]=[CH:13][C:5]=3[O:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:2]=2[CH2:21]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6570Methyl vinyl ketoneHCID 2723922Sodium ethoxideHCID 11321766HCID 11321766、化合物

生成物 1

HCID 22760937HCID 22760937、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of 42 g of the compound 10-keto-10,11-dihydrodibenzo(b,f)-oxepine in 200 ml of dry ethanol a solution of sodiumethoxide (7 g of sodium in 500 ml of ethanol) is added dropwise. After stirring the mixture for 30 minutes 16.2 ml of methylvinylketon in 50 ml of ethanol are added, whereupon the solution is refluxed for 1 hour. The solution is cooled then and poured into 2 N HCl. After extracting into ether, washing the ether layer with water (till neutral) and drying the etherial phase, the solvent is evaporated.

後処理

  1. additionare added, whereupon the solution
  2. temperatureis refluxed for 1 hour
  3. temperatureThe solution is cooled
  4. extractionAfter extracting into ether
  5. washwashing the ether layer with water (till neutral)
  6. customdrying the etherial phase
  7. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-e9c9777d53584b1797a134a5499425cc
出典データセット
uspto-grants-1976_04
特許番号
US03950425

反応ノート

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