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Water → HCID 68153798、化合物

HRID 73613
ノート
印刷プレビュー

反応式

HRID 73613 の反応式
[CH2:1]([N:8]1[C@H:17]2[C@:12]([OH:18])([CH2:13][CH2:14][CH2:15][CH2:16]2)[C:11](OCC)(OCC)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.C12(CS(O)(=O)=O)C(C)(C)C(CC1)CC2=O.C([N:48]1[C@@H:57]2[C@:52](O)([CH2:53][CH2:54][CH2:55][CH2:56]2)C(=O)CC1)C1C=CC=CC=1.NC1C=CC=CC=1.[BH4-].[Na+]>C1(C)C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].CC(O)=O.ClCCCl.CCO>[CH2:1]([N:8]1[C@H:17]2[C@:12]([OH:18])([CH2:13][CH2:14][CH2:15][CH2:16]2)[C@H:11]([NH:48][C:57]2[CH:52]=[CH:53][CH:54]=[CH:55][CH:56]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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

12

反応物 6

HCID 962WaterHCID 6115AnilineHCID 18462Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-HCID 4311764Sodium borohydrideHCID 68154006HCID 68154006、化合物HCID 68154419HCID 68154419、化合物

生成物 1

HCID 68153798
HCID 68153798、化合物

試薬・触媒・溶媒 5

HCID 111,2-Dichloroethane溶媒HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 1140Toluene溶媒HCID 11430Potassium Carbonate溶媒

反応条件

温度
80 °C

実験手順

To (4aR,8aR)-1-benzyl-4,4-diethoxyoctahydroquinolin-4a(2H)-ol (200 mg, 0.600 mmol) in toluene (12.000 ml) at room temperature was added water (0.162 ml, 9.00 mmol) followed by camphorsulfonic acid (153 mg, 0.660 mmol). The reaction mixture was heated to reflux for 3 hrs. The reaction mixture was diluted with aqueous potassium carbonate (saturated, 30 mL). The aqueous layer was extracted with ethyl acetate (3×20 mL). The combined organic fractions were washed with brine (saturated, 30 mL), dried, filtered and the solvent was evaporated under reduced pressure. A mixture of (4aR,8aS)-1-benzyl-4a-hydroxyoctahydroquinolin-4(1H)-one (0.500 g, 1.93 mmol) and aniline (0.528 mL, 5.78 mmol) in 4% CH3COOH in DCE (10 mL) was stirred for 4 hr at 80° C. The reaction was then cooled to rt and NaBH4 (0.438 g, 11.6 mmol) was then added followed by the addition of EtOH (10 mL). The mixture was then stirred overnight at rt. The mixture was then quenched with sat'd. aq. NH4Cl. It was then basified with 2M Na2CO3 and extracted 3× with EtOAc. The combined organics were dried, filtered and concentrated. The residue was purified by column chromatography to give the title compound. 1H-NMR (500 MHz, CDCl3) δ 7.29-7.35 (m, 4H), 7.23-7.30 (m, 1H), 7.17 (t, 2H, J=8.3 Hz), 6.76-6.84 (m, 3H), 4.10 (d, 1H, J=8.0 Hz), 3.96 (d, 1H, J=13.2 Hz), 3.03 (d, 1H, J=13.2 Hz), 2.97 (s, 1H), 2.86 (t, 1H, J=7.8 Hz), 2.37 (d, 1H, J=6.8 Hz), 1.41-2.24 (m, 10H). HRMS (ES) m/z M±H calc'd: 337.2274. found: 337.2275.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 3 hrs
  3. extractionThe aqueous layer was extracted with ethyl acetate (3×20 mL)
  4. washThe combined organic fractions were washed with brine (saturated, 30 mL)
  5. customdried
  6. filtrationfiltered
  7. customthe solvent was evaporated under reduced pressure
  8. temperatureThe reaction was then cooled to rt
  9. stirringThe mixture was then stirred overnight at rt
  10. customThe mixture was then quenched with sat'd
  11. extractionextracted 3× with EtOAc
  12. customThe combined organics were dried
  13. filtrationfiltered
  14. concentrationconcentrated
  15. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-4c0e8fa6552c454ba2fe70678eb2c057
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829196B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート