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Sulfuric Acid → HCID 12822290、化合物

HRID 614274
ノート
印刷プレビュー

反応式

HRID 614274 の反応式
[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([CH:10]2[CH2:13][N:12]([CH3:14])[CH2:11]2)[C:8]#N)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)[OH:22].[OH-:26].[Na+]>>[OH:26][CH2:13][CH:10]1[CH2:11][N:12]([CH3:14])[C:8](=[O:22])[C:7]1([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=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 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 12822283HCID 12822283、化合物

生成物 1

HCID 12822290HCID 12822290、化合物

実験手順

Forty grams (0.153 mole) of α,α-diphenyl-α-(1-methyl-3-azetidinyl)acetonitrile was heated in 150 g. of 70% sulfuric acid solution for 48 hrs. at 130° C. The reaction mixture was poured onto ice and made basic with a 50% sodium hydroxide solution while cooling with the addition of more ice. This mixture was extracted with chloroform, combined extracts dried, filtered, and concentrated in vacuo. The residue was crystallized from toluene, weighed 34.5 g. and melted at 148°-150° C. Ten grams was recrystallized twice from toluene, weighed 7.5 g., and melted at 149°-151° C.

後処理

  1. customat 130° C
addition
The reaction mixture was poured onto ice
  • temperaturewhile cooling with the addition of more ice
  • extractionThis mixture was extracted with chloroform
  • customdried
  • filtrationfiltered
  • concentrationconcentrated in vacuo
  • customThe residue was crystallized from toluene
  • customTen grams was recrystallized twice from toluene
  • 出典と根拠

    ORDレコード
    ord-68e50037ad304b9a88da2ee4376c2dda
    出典データセット
    uspto-grants-1979_03
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04144245

    反応ノート

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