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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
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HRID 345998 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8113Diethanolamine2회HCID 14798Sodium Hydroxide2회HCID 199917602-Chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine2회

생성물 1

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

시약·촉매·용매 2

HCID 962
Water
용매
2회
HCID 7237O-Xylene용매

실험 절차

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°.

후처리

  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°

출처 및 근거

ORD 기록
ord-ef585ad905df4281a6974dd7c49ff092
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05059689

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