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Water → N-[3-(3-Methyl-1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]butanamide

HRID 329640
ノート
印刷プレビュー

反応式

HRID 329640 の反応式
[CH3:1][C:2]1[N:6]2[N:7]=[C:8]([C:11]3[CH:16]=[CH:15][CH:14]=[C:13]([NH2:17])[CH:12]=3)[CH:9]=[CH:10][C:5]2=[N:4][N:3]=1.C(N(C(C)C)CC)(C)C.[C:27](Cl)(=[O:31])[CH2:28][CH2:29][CH3:30].O>ClCCl>[CH3:1][C:2]1[N:6]2[N:7]=[C:8]([C:11]3[CH:12]=[C:13]([NH:17][C:27](=[O:31])[CH2:28][CH2:29][CH3:30])[CH:14]=[CH:15][CH:16]=3)[CH:9]=[CH:10][C:5]2=[N:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8855Butyryl chlorideHCID 81531DiisopropylethylamineHCID 127268683-Methyl-6-[3-(amino)phenyl]-1,2,4-triazolo[4,3-b]pyridazine

生成物 1

HCID 7532414N-[3-(3-Methyl-1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]butanamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

To a solution of 6 g of 3-methyl-6-[3-(amino)-phenyl]-1,2,4-triazolo [4,3-b]pyridazine and 5.1 ml diisopropylethylamine in 500 ml dichloromethane was added 3.1 ml of butyryl chloride. This solution was stirred for 12 hours then poured onto 200 ml of water and extracted with 150 ml portions of dichloromethane. The combined extracts were dried, concentrated in vacuo and the solid chromatographed on 500 g silica gel with dichloromethane-methanol (95:5). The fractions containing the desired product were combined, concentrated in vacuo and the solid recrystalized from dichloromethane-hexane to give.5.58 g of white crystals, mp 195°-198° C.

後処理

  1. extractionextracted with 150 ml portions of dichloromethane
  2. customThe combined extracts were dried
  3. concentrationconcentrated in vacuo
  4. customthe solid chromatographed on 500 g silica gel with dichloromethane-methanol (95:5)
  5. additionThe fractions containing the desired product
  6. concentrationconcentrated in vacuo
  7. customthe solid recrystalized from dichloromethane-hexane
  8. customto give

出典と根拠

ORDレコード
ord-b5f6f74a7e9249b191334411dbb11949
出典データセット
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04892873

反応ノート

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