Ammonium Chloride → HCID 13827615, compound

HRID 1287465Notes

Reaction equation

HRID 1287465 reaction equation
[CH:1]1([C:6]2([CH3:20])[CH2:14][C:13]3[C:8](=[C:9]([Cl:18])[C:10]([Cl:17])=[C:11]([S:15]C)[CH:12]=3)[C:7]2=[O:19])[CH2:5][CH2:4][CH2:3][CH2:2]1.[Na].[Cl-].[NH4+]>N>[CH:1]1([C:6]2([CH3:20])[CH2:14][C:13]3[C:8](=[C:9]([Cl:18])[C:10]([Cl:17])=[C:11]([SH:15])[CH:12]=3)[C:7]2=[O:19])[CH2:2][CH2:3][CH2:4][CH2:5]1

Participants

5

Reactant 3

HCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 203584612-Cyclopentyl-2-methyl-5-methylthio-6,7-dichloro-1-indanone

Product 1

HCID 13827615HCID 13827615, compound

Reagents, catalysts & solvents 1

HCID 222AmmoniaSolvent

Procedure

To a stirred suspension of 2-cyclopentyl-2-methyl-5-methylthio-6,7-dichloro-1-indanone (3.59 g., 0.01 mole) in liquid ammonia (100 ml.) cooled in a dry-ice-acetone bath is added sodium (460 mg., 0.02 gr. atom) in small portions until a permanent blue color persists. Ammonium chloride (1.0 g.) is added, the excess ammonia is evaporated and the reaction mixture is dissolved in water, acidified and extracted with ether which is washed with water, dried over magnesium sulfate and evaporated at reduced pressure affording 2-cyclopentyl-2-methyl-5-mercapto-6,7-dichloro-1-indanone.

Workup

  1. temperaturecooled in a dry-ice-acetone bath
  2. customthe excess ammonia is evaporated
  3. dissolutionthe reaction mixture is dissolved in water
  4. extractionextracted with ether which
  5. washis washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated at reduced pressure

Sources & evidence

ORD record
ord-e35a51ca40274c1585a851c9d69d6e54
Source dataset
uspto-grants-1976_10
Patent number
US03984465

Reaction notes

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