Water → 6-Cyclopropylmethoxy-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine

HRID 657850ノート

反応式

HRID 657850 の反応式
[CH:1]1([CH2:4][OH:5])[CH2:3][CH2:2]1.[H-].[Na+].Br.Cl[C:10]1[CH:11]=[CH:12][C:13]2[N:14]([C:16]([NH2:19])=[N:17][N:18]=2)[N:15]=1.O>CN(C=O)C>[CH:1]1([CH2:4][O:5][C:10]2[CH:11]=[CH:12][C:13]3[N:14]([C:16]([NH2:19])=[N:17][N:18]=3)[N:15]=2)[CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 75644CyclopropanemethanolHCID 866507946-Chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide

生成物 1

HCID 581369646-Cyclopropylmethoxy-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
40 °C

実験手順

Cyclopropylmethanol (2.64 ml) was initially charged in DMF (35 ml), admixed under argon with sodium hydride (795 mg) and stirred at 40° C. for 1 h. Subsequently, 6-chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.001; 1.66 g), dissolved in DMF (35 ml), were added dropwise. After 1 h, the mixture was admixed with water and extracted by shaking four times with dichloromethane. The combined organic phases were dried over magnesium sulfate and concentrated by rotary evaporation. The residue was triturated with MtB ether, filtered off with suction and dried. 720 mg of the title compound were obtained.

後処理

  1. additionwere added dropwise
  2. waitAfter 1 h
  3. extractionextracted
  4. stirringby shaking four times with dichloromethane
  5. dry with materialThe combined organic phases were dried over magnesium sulfate
  6. concentrationconcentrated by rotary evaporation
  7. customThe residue was triturated with MtB ether
  8. filtrationfiltered off with suction
  9. customdried

出典と根拠

ORDレコード
ord-da0f28ff919f4941a8028bc1e32a934a
出典データセット
uspto-grants-2011_12
特許番号
US08076336B2

反応ノート

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