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Hydrazine hydrate (1:1) → 4-(6-Hydrazinylpyrimidin-4-yl)-1,4-oxazepane

HRID 2039482
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인쇄 미리보기

반응식

HRID 2039482 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[N:10]=[CH:9][N:8]=[C:7]([N:11]2[CH2:17][CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH:6]=1>C(O)C>[NH:2]([C:5]1[N:10]=[CH:9][N:8]=[C:7]([N:11]2[CH2:17][CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH:6]=1)[NH2:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 579250744-(6-Chloropyrimidin-4-yl)-1,4-oxazepane

생성물 1

HCID 579250704-(6-Hydrazinylpyrimidin-4-yl)-1,4-oxazepane

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

At RT, 8.8 ml (9.0 g, 180.2 mmol) of hydrazine hydrate are added dropwise with stirring to a solution of 3.9 g (18.0 mmol) of 4-(6-chloropyrimidin-4-yl)-1,4-oxazepane in 25 ml of ethanol. After 16 h of stirring at 80° C., the reaction solution is concentrated under reduced pressure. The residue is triturated with cold ethanol, the precipitated solid is filtered off and the filter residue is washed with 25 ml of diethyl ether. The product is dried under reduced pressure. Yield: 1.4 g (36% of theory)

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후처리

  1. concentrationthe reaction solution is concentrated under reduced pressure
  2. customThe residue is triturated with cold ethanol
  3. filtrationthe precipitated solid is filtered off
  4. washthe filter residue is washed with 25 ml of diethyl ether
  5. customThe product is dried under reduced pressure

출처 및 근거

ORD 기록
ord-cd739734ec2248e0a66815e192b1dd84
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08580778B2

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