Ethyl 2-chloroacetoacetate → HCID 178418931、化合物

HRID 11196

反応式

HRID 11196 の反応式
[NH2:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.C([O:9][C:10](=O)[CH:11]([Cl:15])[C:12]([CH3:14])=O)C>C(O)(=O)C.CCOCC.CO.CN(C=O)C.CS(C)=O>[Cl:15][C:11]1[C:12]([CH3:14])=[N:1][C:2]2[N:3]([N:4]=[CH:5][N:6]=2)[C:10]=1[OH:9]

参加物

7

反応物 2

HCID 11858Ethyl 2-chloroacetoacetateHCID 178418311HCID 178418311、化合物

生成物 1

HCID 178418931HCID 178418931、化合物

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒HCID 679Dimethyl Sulfoxide溶媒HCID 6228Dimethylformamide溶媒HCID 21864698Diethyl ether methanol溶媒

実験手順

3-Amino-1,2,4-triazole (4.2 g, 0.05 mol) and ethyl-2-chloro-acetoacetate (12.64 g, 0.0768 mol) were refluxed in acetic acid (15 ml) under a nitrogen atmosphere. The reaction mixture first turned into a clear yellow solution and after about 15 minutes a solid started precipitating. Reflux continued for one hour. The crude product was filtered off, washed with hot methanol (2×10 ml), and dried in an oven at 90° C. to give 5.9 g (64%) of pure TAI-3. TLC (in Et2O/MeOH, 70:30 v/v) showed only one spot. The compound is soluble in hot DMF and DMSO. mp=starts darkening at ˜308° C. and decomposes at temperatures >325° C.

後処理

  1. customa solid started precipitating
  2. temperatureReflux
  3. waitcontinued for one hour
  4. filtrationThe crude product was filtered off
  5. washwashed with hot methanol (2×10 ml)
  6. customdried in an oven at 90° C.
  7. customto give 5.9 g (64%) of pure TAI-3
  8. customstarts darkening at ˜308° C.
  9. customdecomposes at temperatures >325° C.

出典と根拠

ORDレコード
ord-55ee4330953246a9a99fcfd9784870dc
出典データセット
uspto-grants-2006_08
特許番号
US07097963B1

関連ノート

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