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N,N'-Dimethylethylenediamine → (S)-5-(4-fluoro-phenyl)-6-hydroxymethyl-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one

HRID 2046192
ノート
印刷プレビュー

反応式

HRID 2046192 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][CH:3]=1.[O:9]([CH2:16][C:17]1[CH:32]=[C:20]2[C:21](=[O:31])[NH:22][C@H:23]([CH2:25][O:26][Si](C)(C)C)[CH2:24][N:19]2[N:18]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C([O-])([O-])=O.[K+].[K+].CNCCNC>C1(C)C=CC=CC=1.CCOC(C)=O.[Cu]I>[F:8][C:5]1[CH:6]=[CH:7][C:2]([N:22]2[C@H:23]([CH2:25][OH:26])[CH2:24][N:19]3[N:18]=[C:17]([CH2:16][O:9][C:10]4[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=4)[CH:32]=[C:20]3[C:21]2=[O:31])=[CH:3][CH:4]=1
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

8

反応物 4

HCID 8070N,N'-DimethylethylenediamineHCID 99931-Bromo-4-fluorobenzeneHCID 11430Potassium CarbonateHCID 67976039HCID 67976039、化合物

生成物 1

HCID 67974066(S)-5-(4-fluoro-phenyl)-6-hydroxymethyl-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one収率 71.8%

試薬・触媒・溶媒 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 1140Toluene溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
140 °C

実験手順

Copper (I) iodide (41 mg, 0.22 mmol) was added to a stirred suspension of 4-bromofluorobenzene (0.24 mL, 2.17 mmol), (S)-2-phenoxymethyl-6-trimethylsilanyloxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one (0.37 g, 1.08 mmol), K2CO3 (0.3 g, 2.17 mmol) and N,N′-dimethylethylenediamine (0.070 mL, 0.65 mmol) in toluene (8 mL) in a sealed tube and under nitrogen. The mixture was stirred at 140° C. for 24 hours. The mixture was diluted with AcOEt and washed with a 16% aqueous solution of NH4OH. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo. The residue was dissolved in MeOH (4 mL) and stirred at 100° C. for 10 minutes under microwave irradiation. The solvent was evaporated in vacuo and the residue purified by flash column chromatography (silica; AcOEt in DCM 0/100 to 50/50). Desired fractions were collected and the solvents evaporated in vacuo to yield (S)-5-(4-fluoro-phenyl)-6-hydroxymethyl-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one (285 mg, 71% yield) as an off-white foam. 1H NMR (400 MHz, CDCl3) δ ppm 2.21 (br. s., 1H), 3.57-3.68 (m, 1H), 3.81 (dt, J=10.9, 4.4 Hz, 1H), 4.13-4.20 (m, 1H), 4.61 (dd, J=13.4, 4.9 Hz, 1H), 4.81 (dd, J=13.4, 2.1 Hz, 1H), 5.10 (s, 2H), 6.95-7.03 (m, 4H), 7.09-7.18 (m, 2H), 7.27-7.35 (m, 4H).

後処理

  1. washwashed with a 16% aqueous solution of NH4OH
  2. customThe organic layer was separated
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvents evaporated in vacuo
  6. dissolutionThe residue was dissolved in MeOH (4 mL)
  7. stirringstirred at 100° C. for 10 minutes under microwave irradiation
  8. customThe solvent was evaporated in vacuo
  9. customthe residue purified by flash column chromatography (silica; AcOEt in DCM 0/100 to 50/50)
  10. customDesired fractions were collected
  11. customthe solvents evaporated in vacuo

出典と根拠

ORDレコード
ord-c00831e292cd4cad8610f0788aad389b
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08592422B2

反応ノート

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