Reaction equation
[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([NH:9][C:10]([NH:12][CH2:13][C:14]([F:17])([F:16])[F:15])=S)[CH:6]=[CH:7][CH:8]=1.[NH3:18]>>[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([NH:9][C:10]([NH:12][CH2:13][C:14]([F:17])([F:16])[F:15])=[NH:18])[CH:6]=[CH:7][CH:8]=1Participants
3
Procedure
The above thiourea (1.32 g.) was stirred in 1.6N alcoholic ammonia (50 ml.) with mercuric oxide (3.4 g.) for 17 hours at 20°. The resulting mixture was clarified on the centrifuge and the supernatant was evaporated in vacuo to a syrup which was further dried at 70°/0.1 m.m. to give 1-(3-hydroxymethylphenyl)-3-(2,2,2-trifluoroethyl)guanidine. The n.m.r. spectrum in d6 dimethylsulphoxide using tetramethyl silane as internal standard (δ=0) had the following resonances (δ): 6.9 (4H, multiplet); 4.4 (2H, singlet); 3.9 (2H, quartet).
Workup
- customthe supernatant was evaporated in vacuo to a syrup which
- customwas further dried at 70°/0.1 m
Sources & evidence
- ORD record
- ord-00c69c864a8d46f2b45b9e7a83fcad2d
- Source dataset
- uspto-grants-1988_08
- Patent number
- US04762932
Linked notes
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