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Water → Ethyl 3-(4-tert-butoxycarbonylaminocyclohex-1-enyl)benzoate

HRID 1425296
ノート
印刷プレビュー

反応式

HRID 1425296 の反応式
OC1CCC([C:8]2[CH:18]=[CH:17][CH:16]=[CH:15][C:9]=2[C:10]([O:12][CH2:13][CH3:14])=[O:11])=CC1.CS(Cl)(=O)=O.[N-]=[N+]=[N-].[Na+].O.[C:29]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(O[C:56]([O:58][C:59]([CH3:62])([CH3:61])[CH3:60])=[O:57])(OC(C)(C)C)=O.[N:63]1[CH:68]=[CH:67][CH:66]=[CH:65][CH:64]=1>C(OCC)(=O)C>[C:59]([O:58][C:56]([NH:63][CH:68]1[CH2:67][CH2:66][C:65]([C:18]2[CH:8]=[C:9]([CH:15]=[CH:16][CH:17]=2)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:64][CH2:29]1)=[O:57])([CH3:60])([CH3:61])[CH3:62]
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

9

反応物 7

HCID 962WaterHCID 1049PyridineHCID 11776TriphenylphosphineHCID 31297Methanesulfonyl chlorideHCID 33557Sodium AzideHCID 90495Di-tert-butyl dicarbonateHCID 86648765HCID 86648765、化合物

生成物 1

HCID 67548489
Ethyl 3-(4-tert-butoxycarbonylaminocyclohex-1-enyl)benzoate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒3 回

反応条件

温度
0 °C

実験手順

A solution of ethyl (4-hydroxycyclohex-1-enyl)benzoate obtained in Example (195a) (1 g, 4.06 mmol) in pyridine (20 mL) was cooled to 0° C. Methanesulfonyl chloride (628 μL, 8.12 mmol) was added at the same temperature, and the mixture was stirred at 0° C. for two hours. The reaction solution was diluted with ethyl acetate, washed with 1 N hydrochloric acid and brine, and dried over magnesium sulfate. Thereafter, the solvent was evaporated under reduced pressure. The resulting residue was dissolved in N,N-dimethylformamide (30 mL). Sodium azide (1.32 g, 20.3 mmol) was added at room temperature, and the mixture was stirred at 70° C. for 18 hours. The reaction solution was diluted with ethyl acetate, washed with brine, and dried over magnesium sulfate. Thereafter, the solvent was evaporated under reduced pressure. The resulting residue was dissolved in tetrahydrofuran (30 mL). Water (109 μL, 6.09 mmol) and triphenylphosphine (1.17 g, 4.47 mmol) were added at room temperature, and the mixture was stirred at room temperature for 18 hours. After 18 hours, di-tert-butyl dicarbonate (975 mg, 4.47 mmol) was added, and the mixture was stirred at room temperature for five hours. The reaction solution was diluted with ethyl acetate, washed with brine, and dried over magnesium sulfate. Thereafter, the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=2/1) to obtain 510 g of the title compound as a yellow oily substance (32%).

後処理

  1. washwashed with 1 N hydrochloric acid and brine
  2. dry with materialdried over magnesium sulfate
  3. customThereafter, the solvent was evaporated under reduced pressure
  4. dissolutionThe resulting residue was dissolved in N,N-dimethylformamide (30 mL)
  5. stirringthe mixture was stirred at 70° C. for 18 hours
  6. washwashed with brine
  7. dry with materialdried over magnesium sulfate
  8. customThereafter, the solvent was evaporated under reduced pressure
  9. dissolutionThe resulting residue was dissolved in tetrahydrofuran (30 mL)
  10. stirringthe mixture was stirred at room temperature for 18 hours
  11. waitAfter 18 hours
  12. stirringthe mixture was stirred at room temperature for five hours
  13. washwashed with brine
  14. dry with materialdried over magnesium sulfate
  15. customThereafter, the solvent was evaporated under reduced pressure
  16. customThe resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=2/1)

出典と根拠

ORDレコード
ord-a70e16776c194090acf6d6b92aef5180
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08927588B2

反応ノート

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