Lithium Chloride → 13509-71-2

HRID 371042Notes

Reaction equation

HRID 371042 reaction equation
[CH2:1]([N:8]1[CH2:13][C:12]([CH3:15])([CH3:14])[CH2:11]OC1=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[Li+]>>[CH2:1]([N:8]1[CH2:13][C:12]([CH3:11])([CH3:14])[CH2:15]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

3

Reactant 2

HCID 433294Lithium ChlorideHCID 13175063HCID 13175063, compound

Product 1

HCID 1351960113509-71-2Yield 85%

Conditions

Temperature
245 °C

Procedure

A mixture of 8.97 g (0.04 mole) of tetrahydro-3-benzyl-5,5-dimethyl-1,3-oxazin-2-one and 0.084 g (0.002 mole) of lithium chloride was heated to 245° C. at a pressure of 100 torr in a 25-ml flask equipped with a mechanical stirrer and distillation head. The receiver was cooled with dry ice as the product slowly distilled. After 5 hours, an additional 0.084 g of lithium chloride was added and heating was continued for an additional 25 hours. At this time, 5.84 g (85 percent yield) of pure 1-benzyl-3,3-dimethylazetidine had collected. The material was redistilled at bp 107° C.-108° C. (15 mm).

Workup

  1. customequipped with a mechanical stirrer
  2. distillationdistillation head
  3. temperatureThe receiver was cooled with dry ice as the product
  4. distillationslowly distilled
  5. additionan additional 0.084 g of lithium chloride was added
  6. temperatureheating
  7. waitwas continued for an additional 25 hours

Sources & evidence

ORD record
ord-b1793327fdd6452ba4802a916bde245e
Source dataset
uspto-grants-1985_07
Patent number
US04529544

Reaction notes

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