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Sulfuric Acid → 4-Phenyl-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidine

HRID 1576855
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인쇄 미리보기

반응식

HRID 1576855 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][N:3]=[C:2]1[NH:7][CH2:8][CH2:9][CH:10](O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.S(=O)(=O)(O)O.[OH-].[Na+]>>[C:11]1([CH:10]2[N:3]3[CH2:4][CH2:5][CH2:6][N:1]=[C:2]3[NH:7][CH2:8][CH2:9]2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 21510116HCID 21510116, 화합물

생성물 1

HCID 215101174-Phenyl-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidine

실험 절차

A mixture of 2 parts of α-[2-(1,4,5,6-tetrahydro-2-pyrimidinylamino)ethyl]benzylalcohol and 27 parts of sulfuric acid 80% is stirred for 2 hours at room temperature. The reaction mixture is poured onto crushed ice and the whole is alkalized with sodium hydroxide solution. The product is extracted with toluene. The organic layer is separated, dried, filtered and evaporated. The solid residue is crystallized from acetone, yielding 3,4,6,7,8,9-hexahydro-6-phenyl-2H-pyrimido-[1,2-a]pyrimidine, m.p. 177°-179°C.

후처리

  1. addition
The reaction mixture is poured
  • customonto crushed ice
  • extractionThe product is extracted with toluene
  • customThe organic layer is separated
  • customdried
  • filtrationfiltered
  • customevaporated
  • customThe solid residue is crystallized from acetone
  • 출처 및 근거

    ORD 기록
    ord-02dccde1fa324927a76bc4e1f1c7d368
    출처 데이터셋
    uspto-grants-1976_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US03983133

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