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Hydrazine hydrate (1:1) → N1-(7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl) propane-1,3-diamine

HRID 1921994
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HRID 1921994 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[C:8]([C:28]3[CH:33]=[CH:32][N:31]=[C:30]([NH:34][CH3:35])[N:29]=3)[CH:9]=[C:10]2[NH:13][CH2:14][CH2:15][CH2:16][N:17]2C(=O)C3C(=CC=CC=3)C2=O)=[CH:5][CH:4]=1.O.NN>C(O)C>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[C:8]([C:28]3[CH:33]=[CH:32][N:31]=[C:30]([NH:34][CH3:35])[N:29]=3)[CH:9]=[C:10]2[NH:13][CH2:14][CH2:15][CH2:16][NH2:17])=[CH:5][CH:4]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 532581702-(3-((7-Methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl)amino)propyl)isoindoline-1,3-dione

생성물 1

HCID 67305956N1-(7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl) propane-1,3-diamine

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

To a solution of 2-(3-((7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl) amino)propyl)isoindoline-1,3-dione 181 (95 mg) in ethanol (10 ml) was added hydrazine hydrate (0.1 ml) and the mixture stirred at 80° C. 3 hours. After cooling the mixture in an ice bath the precipitate formed was filtered off and washed with ice cold ethanol. The filtrate was evaporated to dryness to yield N1-(7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl) propane-1,3-diamine 182 as a yellow solid which was used in the next step without further purification.

후처리

  1. custom3 hours
  2. temperatureAfter cooling the mixture in an ice bath the precipitate
  3. customformed
  4. filtrationwas filtered off
  5. washwashed with ice cold ethanol
  6. customThe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-41496f655fb34a70bba45e41c112448f
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08173808B2

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