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Hydrochloric Acid → Ethyl 2-(5-bromo-4-amino-6-oxopyridazin-1(6H)-yl)acetate

HRID 2092080
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인쇄 미리보기

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HRID 2092080 반응식
[Br:1][C:2]1[C:7](=[O:8])[N:6]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[N:5]=[CH:4][C:3]=1[NH:15]CC1C=CC(OCC)=C(OC)C=1.Cl>C(O)C>[Br:1][C:2]1[C:7](=[O:8])[N:6]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[N:5]=[CH:4][C:3]=1[NH2:15]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59574404Ethyl 2-[5-bromo-4-(4-ethoxy-3-methoxybenzylamino)-6-oxopyridazin-1(6H)-yl]acetate

생성물 1

HCID 59574360Ethyl 2-(5-bromo-4-amino-6-oxopyridazin-1(6H)-yl)acetate수율 52%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
90 °C

실험 절차

Ethyl 2-[5-bromo-4-(4-ethoxy-3-methoxybenzylamino)-6-oxopyridazin-1(6H)-yl]acetate (570 mg, 1.29 mmol) in ethanol (11 mL) was stirred with concentrated hydrochloric acid (3.4 mL) at 90° C. for 4 hours. After cooling, the solvent was removed by distillation, and the residue was stirred with ethanol (10 mL) and 4 M hydrogen chloride-1,4-dioxane (1 mL) at 90° C. for 1 hour. After cooling, the solvent was removed by distillation. Toluene was added, and the resulting crystals were collected by filtration as the desired product (184 mg, 52% yield).

후처리

  1. temperatureAfter cooling
  2. customthe solvent was removed by distillation
  3. temperatureAfter cooling
  4. customthe solvent was removed by distillation
  5. additionToluene was added

출처 및 근거

ORD 기록
ord-9f2fb0c160784ca3b5a300ea24d7fd1f
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08440666B2

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