Carbon Dioxide → HCID 53903889, compound

HRID 1078560Notes

Reaction equation

HRID 1078560 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH:14]([CH2:17][C:18](OCC)=[O:19])[NH:13][C:12]=2[CH:23]=1.C(=O)=O.[OH-].[Na+]>O1CCCC1.O.CC(C)=O>[F:7][C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH:14]([CH2:17][CH2:18][OH:19])[NH:13][C:12]=2[CH:23]=1

Participants

8

Reactant 4

HCID 280Carbon DioxideHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 54054098HCID 54054098, compound

Product 1

HCID 53903889HCID 53903889, compound

Reagents, catalysts & solvents 3

HCID 180AcetoneSolventHCID 962WaterSolventHCID 8028TetrahydrofuranSolvent2×

Procedure

145 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, 5.9 g (0.153 mol) of lithium aluminium hydride are added, followed by dropwise addition of 23.22 g (0.097 mol) of ethyl (±)-6-fluoro-3,4-dihydro-2H-1,4-benzoxazine-3-acetate dissolved in 145 ml of tetrahydrofuran, and the mixture is stirred for 2.5 h. The reactor is cooled with a mixture of cardice and acetone, 45 ml of water and 23 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
  2. additionare added dropwise
  3. stirringstirring
  4. waitis continued for 0.5 h.

Sources & evidence

ORD record
ord-c27575a71ac04ddc9f55b251c52a099a
Source dataset
uspto-grants-1996_08
Patent number
US05550125

Reaction notes

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