Chloroform → HCID 86620647, compound

HRID 1157684Notes

Reaction equation

HRID 1157684 reaction equation
[CH3:1][C:2]([NH:4][CH2:5][CH2:6][C:7]1[CH:8]=[C:9]([NH:13][C:14](=[O:17])[O:15][CH3:16])[CH:10]=[CH:11][CH:12]=1)=O.C(Cl)(Cl)Cl.P(Cl)(Cl)(Cl)(Cl)Cl>O>[CH3:1][C:2]1[C:12]2[C:7](=[CH:8][C:9]([NH:13][C:14](=[O:17])[O:15][CH3:16])=[CH:10][CH:11]=2)[CH2:6][CH2:5][N:4]=1

Participants

5

Procedure

A mixture of 4.13 g (17.5 mmol) methyl N-[3-(2-methylcarbonylamino-ethyl)phenyl]carbamate and 35 ml chloroform is slowly combined with 8.00 g (38.4 mmol) phosphorus pentachloride and the mixture is stirred for 16 h. Then the mixture is carefully poured into water and stirred for 45 min. It is extracted 3× with methylene chloride and then the aqueous phase is made basic with 4N NaOH. The crystals precipitated are suction filtered and dried.

Workup

  1. stirringstirred for 45 min
  2. extractionIt is extracted 3× with methylene chloride
  3. customThe crystals precipitated
  4. filtrationare suction filtered
  5. customdried

Sources & evidence

ORD record
ord-d1dceaa090734430a04f703030c28e61
Source dataset
uspto-grants-2010_10
Patent number
US07807693B2

Reaction notes

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