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

HRID 657850노트

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HRID 657850 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-da0f28ff919f4941a8028bc1e32a934a
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076336B2

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