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Hydrochloric Acid → isopropyl 5-benzoyl-7-bromo-1,2-dihydro-3H-pyrrolo[1,2-a]pyrrole-1-carboxylate

HRID 2164650
ノート
印刷プレビュー

反応式

HRID 2164650 の反応式
[C:1]([C:9]1[N:13]2[CH2:14][CH2:15][CH:16]([C:17]([OH:19])=[O:18])[C:12]2=[C:11]([Br:20])[CH:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH:22](O)([CH3:24])[CH3:23]>>[C:1]([C:9]1[N:13]2[CH2:14][CH2:15][CH:16]([C:17]([O:19][CH:22]([CH3:24])[CH3:23])=[O:18])[C:12]2=[C:11]([Br:20])[CH:10]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 155806305-Benzoyl-7-bromo-2,3-dihydro-1H-pyrrolizine-1-carboxylic acid

生成物 1

HCID 20404966isopropyl 5-benzoyl-7-bromo-1,2-dihydro-3H-pyrrolo[1,2-a]pyrrole-1-carboxylate

実験手順

A solution of 1.34 g. of 5-benzoyl-7- bromo-1,2-dihydro- 3H-pyrrolo[1,2-a]pyrrole-1-carboxylic acid in 50 ml. of isopropanol, cooled in an ice bath is saturated with gaseous hydrogen chloride, maintaining the temperature of the reaction mixture below 50° C. The ice bath is then removed and the reaction mixture is stirred for 1.5 hours at room temperature, and evaporated to dryness under reduced pressure; 10 ml. of benzene is added to the residue and the solution is evaporated under vacuum once again, repeating this process a total of three times to completely remove the excess hydrogen chloride, thus obtaining of isopropyl 5-benzoyl-7-bromo-1,2-dihydro-3H-pyrrolo[1,2-a]pyrrole-1-carboxylate. The product is recrystallized from methanol-ethyl acetate.

後処理

  1. temperaturemaintaining the temperature of the reaction mixture below 50° C
  2. customThe ice bath is then removed
  3. customevaporated to dryness under reduced pressure
  4. additionof benzene is added to the residue
  5. customthe solution is evaporated under vacuum once again
  6. customto completely remove the excess hydrogen chloride

出典と根拠

ORDレコード
ord-801fcf2288bb4a35a00c6cc535b43205
出典データセット
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04505927

反応ノート

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