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Water → 1-[3-(2,4,5-Trifluorophenyl)propyl]-3-(4-tert-butoxycarbonyl-1-piperazinyl)-2(1H)-pyrazinone

HRID 1295702
ノート
印刷プレビュー

反応式

HRID 1295702 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:15](=[O:20])[NH:16][CH:17]=[CH:18][N:19]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CC([O-])(C)C.[K+].CS(O[CH2:32][CH2:33][CH2:34][C:35]1[CH:40]=[C:39]([F:41])[C:38]([F:42])=[CH:37][C:36]=1[F:43])(=O)=O.O>C1COCC1.CCOC(C)=O>[F:43][C:36]1[CH:37]=[C:38]([F:42])[C:39]([F:41])=[CH:40][C:35]=1[CH2:34][CH2:33][CH2:32][N:16]1[CH:17]=[CH:18][N:19]=[C:14]([N:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7])[CH2:13][CH2:12]2)[C:15]1=[O:20]
参加物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 962WaterHCID 23665647Potassium tert-butoxideHCID 590138923-(4-tert-Butoxycarbonyl-1-piperazinyl)-2(1H)-pyrazinoneHCID 86591618HCID 86591618、化合物

生成物 1

HCID 693661361-[3-(2,4,5-Trifluorophenyl)propyl]-3-(4-tert-butoxycarbonyl-1-piperazinyl)-2(1H)-pyrazinone収率 86.8%

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
2 回
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 3-(4-tert-butoxycarbonyl-1-piperazinyl)-2(1H)-pyrazinone (obtained in Example 48, Step 1; 0.53 g, 1.91 mmol) in THF (10 mL) was added t-BuOK (0.21 g, 1.91 mmol) and the mixture was stirred at room temperature for 10 min. The resultant mixture was added dropwise to a solution of 3-(2,4,5-trifluorophenyl)propyl methanesulfonate (0.66 g, ˜2.1 mmol; from Step 3) in THF (10 mL). The mixture was stirred at 35° C. for 3 days. Then, the solution was cooled to 0° C. and water (20 mL) and EtOAc (25 mL) were added. The aqueous phase was saturated with NaCl (2 g) and extraction performed. After separation and repeated extraction with EtOAc (15 mL) the combined organic layers were washed with brine and dried over Na2SO4. Concentration in vacuum gave 0.75 g of a yellowish oil which was purified by column chromatography on silica gel using EtOAc/n-hexane (4:1) as eluent. This gave 0.50 g (57%) of the title compound as a colorless oil. HPLC purity: 91%. 1H NMR and MS analyses support the stated structure.

後処理

  1. stirringThe mixture was stirred at 35° C. for 3 days
  2. temperatureThen, the solution was cooled to 0° C.
  3. extractionThe aqueous phase was saturated with NaCl (2 g) and extraction
  4. customAfter separation
  5. extractionextraction with EtOAc (15 mL) the combined organic layers
  6. washwere washed with brine
  7. dry with materialdried over Na2SO4
  8. concentrationConcentration in vacuum

出典と根拠

ORDレコード
ord-4b1b10c182c2489f9e370aefe609275d
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07244722B2

反応ノート

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