Dichloromethane → 2-Pyrrolidinone, 3-chloro-4-(chloromethyl)-1-(phenylmethyl)-

HRID 1834109ノート

反応式

HRID 1834109 の反応式
[CH2:1]([N:4]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:5](=[O:9])[CH:6](Cl)[Cl:7])[CH:2]=[CH2:3].COCCOCCOC.N1CCCC1=O.C(Cl)[Cl:33]>>[CH2:10]([N:4]1[CH2:1][CH:2]([CH2:3][Cl:33])[CH:6]([Cl:7])[C:5]1=[O:9])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 4

HCID 6344DichloromethaneHCID 8150DiglymeHCID 120252-PyrrolidoneHCID 10083827Acetamide, 2,2-dichloro-N-(phenylmethyl)-N-2-propenyl-

生成物 1

HCID 118212562-Pyrrolidinone, 3-chloro-4-(chloromethyl)-1-(phenylmethyl)-

実験手順

Eleven and one-tenth grams of N-allyl-N-benzyl dichloroacetamide was dissolved in 12 ml. of diglyme and 1 g. of anhydrous ferrous chloride added. The mixture was heated at reflux under nitrogen until conversion to the pyrrolidinone was complete as indicated by GLPC. The mixture was diluted with methylene chloride, washed with 5 per cent hydrochloric acid, separated, dried over anhydrous magnesium sulfate, treated with activated carbon and Florisil and stripped under vacuum. Yield was 6 g. of the title compound, nD30 1.5387.

後処理

  1. temperatureThe mixture was heated
  2. washwashed with 5 per cent hydrochloric acid
  3. customseparated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. additiontreated with activated carbon and Florisil

出典と根拠

ORDレコード
ord-6ec93fadb1a84c53ada798b7bce2a59a
出典データセット
uspto-grants-1978_01
特許番号
US04069038

反応ノート

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