Carbon Dioxide → HCID 54517257, compound

HRID 1078563Notes

Reaction equation

HRID 1078563 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:10]=[CH:11][C:12]2[O:17][CH2:16][CH:15]([CH2:18][C:19](OCC)=[O:20])[NH:14][C:13]=2[CH:24]=1.C(=O)=O.[OH-].[Na+]>O1CCCC1.O.CC(C)=O>[CH3:7][O:8][C:9]1[CH:10]=[CH:11][C:12]2[O:17][CH2:16][CH:15]([CH2:18][CH2:19][OH:20])[NH:14][C:13]=2[CH:24]=1

Participants

8

Reactant 4

HCID 280Carbon DioxideHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 53889352HCID 53889352, compound

Product 1

HCID 54517257HCID 54517257, compound

Reagents, catalysts & solvents 3

HCID 180AcetoneSolventHCID 962WaterSolventHCID 8028TetrahydrofuranSolvent2×

Procedure

130 ml of tetrahydrofuran are introduced into a 1 l reactor which is cooled with a mixture of ice and salt and, under an argon atmosphere, 5 g (0.132 mol) of lithium aluminium hydride are added, followed by dropwise addition of 20.73 g (0.0825 mol) of ethyl (±)-6-methoxy-3,4-dihydro-2H-1,4-benzoxazine-3-acetate dissolved in 130 ml of tetrahydrofuran, and the mixture is stirred for 1.5 h. The reactor is cooled with a mixture of cardice and acetone, 40 ml of water and 20 ml of 1N sodium hydroxide are added dropwise and stirring is continued for 0.5 h.

Workup

  1. temperatureis cooled with a mixture of ice and salt and, under an argon atmosphere
  2. additionare added dropwise
  3. stirringstirring
  4. waitis continued for 0.5 h.

Sources & evidence

ORD record
ord-2614b4fc69e6414385b471f8ddcd9d84
Source dataset
uspto-grants-1996_08
Patent number
US05550125

Reaction notes

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