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Guanidine, acetate (1:1) → HCID 14011760、化合物

HRID 986215
ノート
印刷プレビュー

反応式

HRID 986215 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2724684Guanidine, acetate (1:1)HCID 20158301HCID 20158301、化合物

生成物 1

HCID 14011760HCID 14011760、化合物収率 31%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-02c8697aae27430dae147ac67897996b
出典データセット
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04711888

反応ノート

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