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Guanidine, acetate (1:1) → HCID 14011760, 화합물

HRID 986215
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HRID 986215 반응식
[C:1]([O:4][CH:5]([C:9](=O)[CH:10]([CH3:12])[CH3:11])[C:6](=O)[CH3:7])(=[O:3])[CH3:2].C(O)(=O)C.[NH2:18][C:19]([NH2:21])=[NH:20]>CN(C)C=O>[C:1]([O:4][C:5]1[C:9]([CH:10]([CH3:12])[CH3:11])=[N:18][C:19]([NH2:21])=[N:20][C:6]=1[CH3:7])(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2724684Guanidine, acetate (1:1)HCID 20158301HCID 20158301, 화합물

생성물 1

HCID 14011760HCID 14011760, 화합물수율 31%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

A mixture of 3-acetoxy-5-methyl-2,4-hexanedione (5 g, 27 mmol) and guanidine acetate (6.4 g, 54 mmol) in 100 ml dimethylformamide (DMF) was heated at 100° C. for 3 hours. After cooling, the concentrated reaction was filtered through a pad of silica gel using an eluent consisting of equal volume parts of hexane and ethylacetate. The filtrate was concentrated and the residue was treated with excess acetic anhydride in the presence of triethylamine. The reaction mixture was concentrated and the residue was crystallized from boiling hexane to yield 1.7 g (31%) 5-acetoxy-2-amino4-isopropyl-6-methylpyrimidine, m.p. 141°-142° C.

후처리

  1. temperatureAfter cooling
  2. customthe concentrated reaction
  3. filtrationwas filtered through a pad of silica gel using an eluent
  4. concentrationThe filtrate was concentrated
  5. additionthe residue was treated with excess acetic anhydride in the presence of triethylamine
  6. concentrationThe reaction mixture was concentrated
  7. customthe residue was crystallized

출처 및 근거

ORD 기록
ord-02c8697aae27430dae147ac67897996b
출처 데이터셋
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04711888

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