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Diethanolamine → 2-[Bis-(2-hydroxyethyl)-amino]-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

HRID 345998
ノート
印刷プレビュー

反応式

HRID 345998 の反応式
[NH:1]([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4].[OH-].[Na+].Cl[C:11]1[N:16]=[C:15]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[N:14]=[C:13]([N:23]2[C:28]([CH3:30])([CH3:29])[CH2:27][C:26]3([O:34][CH2:33][CH2:32][O:31]3)[CH2:25][C:24]2([CH3:36])[CH3:35])[N:12]=1>O.C1(C)C(C)=CC=CC=1>[OH:4][CH2:3][CH2:2][N:1]([CH2:5][CH2:6][OH:7])[C:11]1[N:16]=[C:15]([N:17]2[CH2:18][CH2:19][O:20][CH2:21][CH2:22]2)[N:14]=[C:13]([N:23]2[C:24]([CH3:36])([CH3:35])[CH2:25][C:26]3([O:31][CH2:32][CH2:33][O:34]3)[CH2:27][C:28]2([CH3:30])[CH3:29])[N:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8113Diethanolamine2 回HCID 14798Sodium Hydroxide2 回HCID 199917602-Chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine2 回

生成物 1

HCID 199917692-[Bis-(2-hydroxyethyl)-amino]-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
2 回
HCID 7237O-Xylene溶媒

実験手順

5.3 g of diethanolamine and a solution of 1 g of NaOH in 3 ml of water are added to a solution of 20 g of 2-chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (product from Example 44) in 50 ml of xylene. 1 g of NaOH in 3 ml of water is again added after 1.75 hours with stirring under reflux. After 14 hours, 7.9 g of diethanolamine are added, after which the mixture is stirred under reflux for a further 28 hours. It is then allowed to cool and washed with water, and the organic phase is separated off. After drying over Na2SO4, evaporating and recrystallizing twice from toluene, the above product is obtained as a white powder which melts at 135°-140°.

後処理

  1. temperatureunder reflux
  2. stirringafter which the mixture is stirred
  3. temperatureunder reflux for a further 28 hours
  4. temperatureto cool
  5. washwashed with water
  6. customthe organic phase is separated off
  7. dry with materialAfter drying over Na2SO4
  8. customevaporating
  9. customrecrystallizing twice from toluene
  10. customthe above product is obtained as a white powder which melts at 135°-140°

出典と根拠

ORDレコード
ord-ef585ad905df4281a6974dd7c49ff092
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05059689

反応ノート

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