3-Azabicyclo[3.2.2]nonane → 3-{4,6-Bis[(1,1,2,2-tetramethylpropyl)amino]-s-triazin-2-yl}-3-azabicyclo[3.2.2]nonane

HRID 443758

반응식

HRID 443758 반응식
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]([CH3:15])([CH3:14])[C:10]([CH3:13])([CH3:12])[CH3:11])[N:5]=[C:4]([NH:16][C:17]([CH3:23])([CH3:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[N:3]=1.[CH:24]12[CH2:32][CH2:31][CH:28]([CH2:29][CH2:30]1)[CH2:27][NH:26][CH2:25]2>COCCOCCOC>[CH3:22][C:17]([NH:16][C:4]1[N:5]=[C:6]([NH:8][C:9]([CH3:15])([CH3:14])[C:10]([CH3:13])([CH3:12])[CH3:11])[N:7]=[C:2]([N:26]2[CH2:27][CH:28]3[CH2:31][CH2:32][CH:24]([CH2:30][CH2:29]3)[CH2:25]2)[N:3]=1)([CH3:23])[C:18]([CH3:21])([CH3:20])[CH3:19]

참가 물질

4

반응물 2

HCID 92403-Azabicyclo[3.2.2]nonaneHCID 155725772-Chloro-4,6-di(2,3,3-trimethyl-2-butyl)amino-s-triazine

생성물 1

HCID 99544153-{4,6-Bis[(1,1,2,2-tetramethylpropyl)amino]-s-triazin-2-yl}-3-azabicyclo[3.2.2]nonane

시약·촉매·용매 1

HCID 8150Diglyme용매

실험 절차

A 10.25 g. portion of 2-chloro-4,6-bis[(1,1,2,2-tetramethylpropyl)amino]-s-triazine and 7.65 g. of 3-azabicyclo[3.2.2]nonane in 50 ml. of diglyme is heated at reflux for 3 hours and then cooled, giving a pink solid. This solid is collected, washed with diglyme, suspended in 500 ml. of water, stirred, filtered and washed with water giving a pink solid. This solid is recrystallized from ethanol (charcoal being employed in decolorization) to give the desired product m.p. 282°-284° C.

후처리

  1. temperatureat reflux for 3 hours
  2. temperaturecooled
  3. customgiving a pink solid
  4. customThis solid is collected
  5. washwashed with diglyme
  6. filtrationfiltered
  7. washwashed with water giving a pink solid
  8. customThis solid is recrystallized from ethanol (charcoal being employed in decolorization)

출처 및 근거

ORD 기록
ord-63c0f65b6203474dad71419269b4f029
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04261892

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