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Sulfuric Acid → HCID 12822290, 화합물

HRID 614274
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HRID 614274 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 12822283HCID 12822283, 화합물

생성물 1

HCID 12822290HCID 12822290, 화합물

실험 절차

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.

후처리

  1. customat 130° C
  • additionThe 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
  • 출처 및 근거

    ORD 기록
    ord-68e50037ad304b9a88da2ee4376c2dda
    출처 데이터셋
    uspto-grants-1979_03
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04144245

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