4-Fluorobenzene-1,2-diamine → HCID 22139847, compound

HRID 2250482Notes

Reaction equation

HRID 2250482 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([NH2:9])[CH:3]=1.[CH3:10][C:11]1[C:12]([N:16]=[C:17]=[S:18])=[CH:13][S:14][CH:15]=1>C1COCC1>[NH2:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][C:4]=1[NH:9][C:17]([NH:16][C:12]1[C:11]([CH3:10])=[CH:15][S:14][CH:13]=1)=[S:18]

Participants

4

Procedure

0.02 mol of 4-fluoro-1,2-diaminobenzene is added to a solution of 0.02 mol of 4-methyl-3-thienyl isothiocyanate in 60 ml of anhydrous THF. The reaction mixture is stirred at room temperature for 2 hours and then allowed to stand overnight, and the solvent is then distilled off under reduced pressure using a rotary evaporator and the oily residue is purified on a silica gel column using a mixture of identical proportions of toluene and ethyl acetate.

Workup

  1. waitto stand overnight
  2. distillationthe solvent is then distilled off under reduced pressure
  3. customa rotary evaporator
  4. customthe oily residue is purified on a silica gel column
  5. additiona mixture of identical proportions of toluene and ethyl acetate

Sources & evidence

ORD record
ord-7136761aba234e38bebb15cd9dc9c028
Source dataset
uspto-grants-2008_01
Patent number
US07317033B2

Reaction notes

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