Water → HCID 22759921, compound

HRID 1703758Notes

Reaction equation

HRID 1703758 reaction equation
[H-].[H-].[H-].[H-].[Li+].[Al+3].[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[O:17][CH2:16][CH2:15][N:14]=[C:13]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:12]=2[CH:24]=1.O.[OH-].[Na+]>C(OCC)C>[ClH:7].[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[O:17][CH2:16][CH2:15][NH:14][CH:13]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:12]=2[CH:24]=1

Participants

6

Reactant 4

HCID 962Water2×HCID 14798Sodium HydroxideHCID 13221358HCID 13221358, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 22759921HCID 22759921, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

To a stirred suspension of 64.3 g (1.69 moles) of LiAlH4 in 1500 ml of anhydrous diethyl ether was added a solution of 144.0 g (0.537 mole) of crude 7-chloro-2,3-dihydro-5-phenyl-1,4-benzoxazepine produced in step (b) in 1000 ml of anhydrous diethyl ether, at a rate sufficient to maintain reflux. The mixture was initially blue, changing to a dark green which lightened with time. After addition was complete the mixture was stirred and refluxed for two hours. The reaction mixture was cooled and cautiously decomposed by the dropwise addition of 64.2 ml of water, followed by 64.2 ml of 15% NaOH solution and finally 192.6 ml of water. Stirring was continued for 30 minutes and then the inorganic solid was filtered off. The filter cake was washed well with diethyl ether and the combined filtrate and washings were dried over anhydrous Na2SO4.

Workup

  1. temperatureat a rate sufficient to maintain
  2. temperaturereflux
  3. additionAfter addition
  4. temperaturerefluxed for two hours
  5. temperatureThe reaction mixture was cooled
  6. stirringStirring
  7. filtrationthe inorganic solid was filtered off
  8. washThe filter cake was washed well with diethyl ether
  9. dry with materialthe combined filtrate and washings were dried over anhydrous Na2SO4

Sources & evidence

ORD record
ord-2c9711a1a2f848b4a35d87fa023ce555
Source dataset
uspto-grants-1978_11
Patent number
US04125538

Reaction notes

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