Ammonia → 3,3-Diphenyl-2-pyrrolidinone

HRID 1667061

反応式

HRID 1667061 の反応式
[C:1]1([C:7]2([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH2:11][CH2:10][O:9][C:8]2=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH3:19]>[Cl-].[Zn+2].[Cl-].C(O)C>[C:1]1([C:7]2([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH2:11][CH2:10][NH:19][C:8]2=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 2

HCID 222Ammonia2 回HCID 70393Dihydro-3,3-diphenyl-2(3H)-furanone

生成物 1

HCID 2382533,3-Diphenyl-2-pyrrolidinone

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 702Ethanol溶媒

反応条件

温度
225 °C

実験手順

3,3-Diphenyldihydrofuran-2(3H)-one (3.98 g, 16.70 mmol) and zinc chloride (0.080 g) were placed in an autoclave. Ammonia (8 mL) was added, and the reactor was sealed and heated at 225° C. for 21 hours under an argon atmosphere at an equilibrium pressure of 800 pounds per square inch. The vessel was cooled, the ammonia was vented, and a mixture of solids was obtained. The solid was treated with ethanol (100 mL), filtered and concentrated. Silica gel chromatography eluting with 5% methanol/dichloromethane gave the title compound. MS (DCI+) m/z 238.1 (M+H)+.

後処理

  1. customthe reactor was sealed
  2. temperatureThe vessel was cooled
  3. additiona mixture of solids
  4. customwas obtained
  5. filtrationfiltered
  6. concentrationconcentrated
  7. washSilica gel chromatography eluting with 5% methanol/dichloromethane

出典と根拠

ORDレコード
ord-11a05090fd12422c8e019d8a70dd8476
出典データセット
uspto-grants-2011_10
特許番号
US08044069B2

関連ノート

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