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

HRID 1031877
ノート
印刷プレビュー

反応式

HRID 1031877 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 222AmmoniaHCID 22166509HCID 22166509、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3d8c08db2a8046a0b89321b203047022
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04956367

反応ノート

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