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Ammonia → Ethanol, 2-((4-(4-morpholinyl)-6-propyl-1,3,5-triazin-2-yl)amino)-, carbamate (ester)

HRID 1031871
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HRID 1031871 반응식
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:12]=[C:11]([NH:13][CH2:14][CH2:15][O:16][C:17](OC3C=CC=CC=3)=[O:18])[N:10]=[C:9]([CH2:26][CH2:27][CH3:28])[N:8]=2)[CH2:3][CH2:2]1.[NH3:29]>ClCCl>[NH2:29][C:17]([O:16][CH2:15][CH2:14][NH:13][C:11]1[N:12]=[C:7]([N:4]2[CH2:5][CH2:6][O:1][CH2:2][CH2:3]2)[N:8]=[C:9]([CH2:26][CH2:27][CH3:28])[N:10]=1)=[O:18]
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참가 물질

4

반응물 2

HCID 222AmmoniaHCID 22166509HCID 22166509, 화합물

생성물 1

HCID 3080163Ethanol, 2-((4-(4-morpholinyl)-6-propyl-1,3,5-triazin-2-yl)amino)-, carbamate (ester)수율 97.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

19.4 g (0.05 mole) of 2-morpholino-4-[[2-[(phenoxycarbonyl)oxy]ethyl]amino]-6-propyl-1,3,5-triazine, dissolved in 100 ml of anhydrous dichloromethane are introduced into one liter of liquid ammonia. Stirring is continued for 7 hours at a temperature of between -35° C. and -45° C. The ammonia is then evaporated and the organic phase is washed successively with an aqueous solution of sodium bicarbonate and with water. It is dried over sodium sulfate and the solvent is evaporated under reduced pressure. The residue obtained crystallizes in a 50:50 mixture (v/v) of ethyl acetate-hexane. 15.1 g of 2-[[2-[(aminocarbonyl)oxy]ethyl]amino]-4-morpholino-6-propyl-1,3,5-triazine are obtained.

후처리

  1. customThe ammonia is then evaporated
  2. washthe organic phase is washed successively with an aqueous solution of sodium bicarbonate and with water
  3. dry with materialIt is dried over sodium sulfate
  4. customthe solvent is evaporated under reduced pressure
  5. customThe residue obtained
  6. customcrystallizes in a 50:50 mixture (v/v) of ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-2fc833cc15fc430986ea067a23254240
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04956363

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