HCID 12668848, compound → HCID 13326916, compound

HRID 980847Notes

Reaction equation

HRID 980847 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH3:20])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:4][C:3]=1[NH2:21].CS[C:24](SC)=[N:25][C:26](=[O:29])[O:27][CH3:28]>O1CCCC1>[CH2:18]([C:15]1[CH:16]=[CH:17][C:12]([S:9]([O:8][C:5]2[CH:6]=[CH:7][C:2]3[N:1]=[C:24]([NH:25][C:26]([O:27][CH3:28])=[O:29])[NH:21][C:3]=3[CH:4]=2)(=[O:11])=[O:10])=[CH:13][CH:14]=1)[CH2:19][CH3:20]

Participants

4

Reactant 2

HCID 12668848HCID 12668848, compoundHCID 20221110HCID 20221110, compound

Product 1

HCID 13326916HCID 13326916, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

30.6 g of 1,2-diamino-4-(4-propylphenylsulfonyloxy)benzene (see Example 5) and 17.9 g of methyl N-[bis(methylthio)methylene]carbamate in 200 ml of tetrahydrofuran are heated to reflux for four hours. After cooling, the precipitate is filtered off with suction and washed with diisopropyl ether. For purification, it is dissolved in hot dimethylformamide, methanol is added and, after cooling, the product is filtered off with suction, melting point 160° C., decomposition.

Workup

  1. temperatureto reflux for four hours
  2. temperatureAfter cooling
  3. filtrationthe precipitate is filtered off with suction
  4. washwashed with diisopropyl ether
  5. customFor purification, it
  6. dissolutionis dissolved in hot dimethylformamide
  7. additionmethanol is added
  8. temperatureafter cooling
  9. filtrationthe product is filtered off with suction, melting point 160° C., decomposition.

Sources & evidence

ORD record
ord-8e67f83c2c6148b68b38de253fe4785e
Source dataset
uspto-grants-1987_01
Patent number
US04639463

Reaction notes

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