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Sodium Sulfate → Trans-4,6,6a,8,9,10a-hexahydro-1-methoxy-7-methyl-10a-methyl-7H-indolo[3,4-gh][1,4]benzoxazine

HRID 129238
ノート
印刷プレビュー

反応式

HRID 129238 の反応式
[CH3:1][N:2]1[C@@H:7]2[CH2:8][C:9]3[C:10]4[C:15]([N:16](S(C5C(C(C)C)=CC(C(C)C)=CC=5C(C)C)(=O)=O)[CH:17]=3)=[CH:14][CH:13]=[C:12]([O:36][CH3:37])[C:11]=4[C@@:6]2([CH3:38])[O:5][CH2:4][C:3]1=O.[H-].[H-].[H-].[H-].[Li+].[Al+3].S([O-])([O-])(=O)=O.[Na+].[Na+].[Na].C1C2C(=CC=CC=2)C=CC=1.[Cl-].[NH4+]>C1COCC1.C(O)C>[CH3:37][O:36][C:12]1[C:11]2[C@@:6]3([CH3:38])[O:5][CH2:4][CH2:3][N:2]([CH3:1])[C@@H:7]3[CH2:8][C:9]3[C:10]=2[C:15]([NH:16][CH:17]=3)=[CH:14][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 24436Sodium SulfateHCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 54326336trans-4,6,6a,7,9,10a-Hexahydro-7-methyl-10a-methyl-1-methoxy-4-(2,4,6-triisopropylphenylsulfonyl)-indolo[3,4-gh][1,4]benzoxazin-8-oneHCID 66588811Naphthalene sodium

生成物 1

HCID 22857199
Trans-4,6,6a,8,9,10a-hexahydro-1-methoxy-7-methyl-10a-methyl-7H-indolo[3,4-gh][1,4]benzoxazine
収率 27%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a solution of trans-4,6,6a,7,9,10a-hexahydro-7-methyl-10a-methyl-1-methoxy-4-(2,4,6-triisopropylphenylsulfonyl)-indolo[3,4-gh][1,4]benzoxazin-8-one (1.9 g, 3.4 mmol) in THF (30 ml) was added, while stirring under ice-cooling, LAH (3 equivalents). The mixture was heated for 3 hours under reflux. After completion of the reaction, ethanol was added to the reaction mixture, and the mixture was then added to an ice-cooled saturated aqueous solution of sodium sulfate. The mixture was subjected to extraction with ethyl acetate. The extract was washed with an aqueous saline solution, and was then dried (anhydrous sodium sulfate). The solvent was distilled off under reduced pressure. The residue was subjected to a silica gel column chromatography, eluting with ethyl acetate to leave 700 mg of a residual substance. To a solution of this residual substance in THF (10 ml) was added, at room temperature in argon streams, a solution of 0.5M naphthalene sodium in THF (10 equivalents). The mixture was stirred for 10 minutes at room temperature, and was added to an ice-cooled saturated aqueous solution of ammonium chloride, followed by extraction with ethyl acetate. The organic layer was washed with an aqueous saline solution, which was dried (anhydrous sodium sulfate). The solvent was distilled off under reduced pressure. The residue was subjected to a silica gel column chromatography, eluting with ethyl acetate to afford 250 mg (27%) of the title compound as crystals, m.p.200°-202° C. (isopropyl ether-ethyl acetate).

後処理

  1. temperaturecooling
  2. temperatureThe mixture was heated for 3 hours
  3. temperatureunder reflux
  4. additionwas added to the reaction mixture
  5. extractionThe mixture was subjected to extraction with ethyl acetate
  6. washThe extract was washed with an aqueous saline solution
  7. dry with materialwas then dried (anhydrous sodium sulfate)
  8. distillationThe solvent was distilled off under reduced pressure
  9. washeluting with ethyl acetate
  10. customto leave 700 mg of a residual substance
  11. stirringThe mixture was stirred for 10 minutes at room temperature
  12. extractionfollowed by extraction with ethyl acetate
  13. washThe organic layer was washed with an aqueous saline solution, which
  14. dry with materialwas dried (anhydrous sodium sulfate)
  15. distillationThe solvent was distilled off under reduced pressure
  16. washeluting with ethyl acetate

出典と根拠

ORDレコード
ord-4f970c408a67456ebb9ff29015cefa3d
出典データセット
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05466689

反応ノート

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