Sodium Sulfate → HCID 22381739, compound

HRID 895776Notes

Reaction equation

HRID 895776 reaction equation
[CH2:1]1[N:12]2[C:13]3[C:9]([C:10]4[CH2:16][CH2:15][CH2:14][C:11]=42)=[CH:8][CH:7]=[CH:6][C:5]=3[CH2:4][NH:3][C:2]1=O.[O-]S([O-])(=O)=O.[Na+].[Na+]>CCOCC.[H-].[H-].[H-].[H-].[Li+].[Al+3]>[CH:1]1[N:12]2[C:13]3[C:9]([C:10]4[CH2:16][CH2:15][CH2:14][C:11]=42)=[CH:8][CH:7]=[CH:6][C:5]=3[CH2:4][NH:3][CH:2]=1

Participants

5

Reactant 2

HCID 24436Sodium SulfateHCID 22381731HCID 22381731, compound

Product 1

HCID 22381739HCID 22381739, compoundYield 70%

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolvent3×HCID 21226445Aluminium lithium hydrideSolvent

Procedure

To a suspension of 3,4,9,10-tetrahydro-8H-cyclopenta[b][1,4]diazepino[6,7,1-hi]indol-2(1H)-one (67 mg, 0.30 mmol) in Et2O (7 mL), LAH power (28 mg, 0.74 mmol) was added slowly at rt under Ar. After 16 h, additional Et2O (5 mL) was added followed by dropwise addition of a sat'd Na2SO4 solution (0.1 mL). H2 gas evolved upon addition. Additional Et2O (8 mL) was added, dried over Na2SO4, filtered and concentrated in vacuo to give 44 mg (70%) of the title compound as a yellow syrup.

Workup

  1. additionwas added slowly at rt under Ar
  2. additionH2 gas evolved upon addition
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-e9935e178cea48f0965b18e469cc2e5d
Source dataset
uspto-grants-2005_07
Patent number
US06916922B2

Reaction notes

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