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Triethylamine → 1-ethyl-6-nitro-N-(3-hydroxycyclohexylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine

HRID 375889
ノート
印刷プレビュー

反応式

HRID 375889 の反応式
[CH2:1]([N:3]1[C:7]2=[N:8][C:9]3[C:14]([C:15](Cl)=[C:6]2[CH:5]=[N:4]1)=[CH:13][C:12]([N+:17]([O-:19])=[O:18])=[CH:11][CH:10]=3)[CH3:2].C(N(CC)CC)C.[OH:27][CH:28]1[CH2:33][CH2:32][CH2:31][CH:30]([CH2:34][NH2:35])[CH2:29]1.[NH4+].[OH-]>C1COCC1.CS(C)=O>[CH2:1]([N:3]1[C:7]2=[N:8][C:9]3[C:14]([C:15]([NH:35][CH2:34][CH:30]4[CH2:31][CH2:32][CH2:33][CH:28]([OH:27])[CH2:29]4)=[C:6]2[CH:5]=[N:4]1)=[CH:13][C:12]([N+:17]([O-:19])=[O:18])=[CH:11][CH:10]=3)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 14923Ammonium HydroxideHCID 212177131-ethyl-4-chloro-6-nitro-1H-pyrazolo[3,4-b]quinolineHCID 230098443-(Aminomethyl)cyclohexan-1-ol

生成物 1

HCID 212177071-ethyl-6-nitro-N-(3-hydroxycyclohexylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine収率 10.5%

試薬・触媒・溶媒 2

HCID 679
Dimethyl Sulfoxide
溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
110 °C

実験手順

A mixture of 1-ethyl-6-nitro-4-chloro-1H-pyrazolo[3,4-b]quinoline (2.7 g, 17.8 mmol), triethylamine (3 mL, 0.02 mol), DMSO (15 mL) and 3-hydroxycyclohexylmethylamine (4.97 g, 18 mmol) was heated at 110° C. overnight. The reaction mixture was poured into ice-water (200 mL)/NH4OH (10 mL) and the solid which formed was collected by filtration. The filtrate was then extracted with CH2Cl2 (2×100 mL). The solid was stirred and sonicated with CH2Cl2 (2×200 mL) and any solids which did not go into solution were collected by filtration. All of the above CH2Cl2 filtrates and extracts were combined, washed with water and evaporated. The residue was slurried with ethyl acetate (10-15 mL)/ether (20 mL) and a red colored solid was collected by filtration and washed with ether. The solid was purified by column chromatography (2×) on silica gel (note that the solid was preloaded onto 50-100 g of silica gel) eluting with 40% THF/cyclohexane and each of the diastereomers which was isolated was dissolved in hot THF, filtered and the solvent was evaporated. Each of the residues was slurried with ethanol (5 mL), filtered and dried to afford 0.69 g of 1-ethyl-6-nitro-N-(3-hydroxycyclohexylmethyl)-1 H-pyrazolo[3,4-b]quinolin-4-amine (the RS,SR diastereomer which is labelled as Example 36(a)), m.p. 236°-238° C. and 2.23 g of 1-ethyl-6-nitro-N-(3-hydroxycyclohexylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine (the RR,SS diastereomer which is labelled as Example 36(b)), m.p. 247°-248° C.

後処理

  1. customthe solid which formed
  2. filtrationwas collected by filtration
  3. extractionThe filtrate was then extracted with CH2Cl2 (2×100 mL)
  4. customsonicated with CH2Cl2 (2×200 mL)
  5. filtrationwere collected by filtration
  6. washwashed with water
  7. customevaporated
  8. filtrationa red colored solid was collected by filtration
  9. washwashed with ether
  10. customThe solid was purified by column chromatography (2×) on silica gel (note that the solid
  11. washeluting with 40% THF/cyclohexane
  12. customeach of the diastereomers which was isolated
  13. filtrationfiltered
  14. customthe solvent was evaporated
  15. filtrationfiltered
  16. customdried

出典と根拠

ORDレコード
ord-4c6eff6cfaa94790a1a4eda7d2469d47
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05488055

反応ノート

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