HCID 12761817, compound → HCID 12761816, compound

HRID 1763905Notes

Reaction equation

HRID 1763905 reaction equation
Cl.[CH3:2][N:3]([CH3:21])[S:4](=[O:20])(=[O:19])[O:5][C:6]1[C:11]([I:12])=[CH:10][C:9]([C:13]([CH3:16])([CH3:15])[CH3:14])=[CH:8][C:7]=1[CH2:17][NH2:18]>O>[CH3:21][N:3]([CH3:2])[S:4](=[O:19])(=[O:20])[O:5][C:6]1[C:11]([I:12])=[CH:10][C:9]([C:13]([CH3:16])([CH3:15])[CH3:14])=[CH:8][C:7]=1[CH2:17][NH2:18]

Participants

3

Conditions

Temperature
20 °C

Procedure

To a solution of 2-aminomethyl-4-(1,1-dimethylethyl)-6-iodophenyl N,N-dimethylsulfamate hydrochloride (100 mg., 0.22 millimole) in water (30 ml.) is added 15N ammonium hydroxide (1 ml.). The resulting heterogeneous mixture is stirred at 20° C. for 5 minutes and decanted. Trituration of the insoluble gummy residue with petroleum ether provides a colorless solid which is collected, washed with petroleum ether and dried to afford 65 mg. (73%) of 2-aminomethyl-4-(1,1-dimethylethyl)-6-iodophenyl N,N-dimethyl sulfamate, m.p. 94°-95° C.

Workup

  1. customdecanted
  2. customTrituration of the insoluble gummy residue with petroleum ether provides a colorless solid which
  3. customis collected
  4. washwashed with petroleum ether
  5. customdried
  6. customto afford 65 mg

Sources & evidence

ORD record
ord-452484d643b44b919d06a386962b5ee1
Source dataset
uspto-grants-1978_09
Patent number
US04113877

Reaction notes

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