1,3-Butanedione, 4,4,4-trifluoro-1-(3-pyridinyl)- → HCID 13309053、化合物

HRID 326093

反応式

HRID 326093 の反応式
[NH2:1][C:2]1[N:6]=[C:5]([CH3:7])[NH:4][N:3]=1.[F:8][C:9]([F:22])([F:21])[C:10](=O)[CH2:11][C:12]([C:14]1[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=1)=O>C(O)(=O)C>[CH3:7][C:5]1[N:6]=[C:2]2[N:1]=[C:10]([C:9]([F:22])([F:8])[F:21])[CH:11]=[C:12]([C:14]3[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=3)[N:3]2[N:4]=1

参加物

4

反応物 2

HCID 684951,3-Butanedione, 4,4,4-trifluoro-1-(3-pyridinyl)-HCID 2346103-Amino-5-methyl-4H-1,2,4-triazole

生成物 1

HCID 13309053HCID 13309053、化合物収率 47.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A reaction mixture of 0.986 g of 3-amino-5-methyl-1,2,4-triazole and 2.178 g of 4,4,4-trifluoro-1-(3-pyridyl)-1,3-butanedione in 25 ml of glacial acetic acid was refluxed for 4 hours. The mixture was then evaporated to dryness in vacuo and gave a crystalline residue. This residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane and the procedure of Example 1 was continued to give 1.33 g of the desired product as colorless crystals, mp 195°-197° C.

後処理

  1. temperaturewas refluxed for 4 hours
  2. customThe mixture was then evaporated to dryness in vacuo
  3. customgave a crystalline residue
  4. customThis residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane

出典と根拠

ORDレコード
ord-55b027c0f6054b40b6bacef41597db46
出典データセット
uspto-grants-1984_04
特許番号
US04444774

関連ノート

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