Sodium sulfate decahydrate → HCID 86697504, compound

HRID 1528291Notes

Reaction equation

HRID 1528291 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].C([O:9][C:10](=O)[CH2:11][N:12]1[C@H:21]2[C@@H:16]([CH2:17][CH2:18][CH2:19][CH2:20]2)[NH:15][C:14](=O)[CH2:13]1)C.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCOCC1>[N:12]1([CH2:11][CH2:10][OH:9])[C@H:21]2[C@@H:16]([CH2:17][CH2:18][CH2:19][CH2:20]2)[NH:15][CH2:14][CH2:13]1

Participants

5

Reactant 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 86697505HCID 86697505, compound

Product 1

HCID 86697504HCID 86697504, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

Lithium aluminum hydride (1.00 g, 26.4 mmol) was suspended in anhydrous dioxane (40 ml). To the suspension, an anhydrous dioxane (10 ml) solution of (trans-3-oxodecahydroquinoxalin-1-yl)acetic acid ethyl ester (2.35 g, 9.78 mmol) was added dropwise with stirring at room temperature, and the mixture was then stirred under reflux for 10 minutes. The reaction mixture was cooled on ice, and sodium sulfate decahydrate was added thereto in small portions until no gas was generated. This mixture was filtered through celite and washed with methylene chloride, and the filtrate was then concentrated under reduced pressure to obtain 2-(trans-decahydroquinoxalin-1-yl)ethanol (1.74 g, yield: 97%) in a brown oil form.

Workup

  1. stirringthe mixture was then stirred
  2. temperatureunder reflux for 10 minutes
  3. additionwas added
  4. filtrationThis mixture was filtered through celite
  5. washwashed with methylene chloride
  6. concentrationthe filtrate was then concentrated under reduced pressure

Sources & evidence

ORD record
ord-281435169f09466d938af89532375f35
Source dataset
uspto-grants-2015_07
Patent number
US09090572B2

Reaction notes

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