Methylhydrazine → HCID 178481943, compound
Reaction equation
C([O:3][C:4](=O)[CH:5]=[C:6](OC)[C:7]([F:13])([F:12])[C:8]([F:11])([F:10])[F:9])C.[CH3:17][NH:18][NH2:19]>>[F:12][C:7]([F:13])([C:6]1[N:18]([CH3:17])[N:19]=[C:4]([OH:3])[CH:5]=1)[C:8]([F:11])([F:10])[F:9]Participants
3
Procedure
62.03 g (0.25 mol) of 3-methoxy-3-pentafluoroethyl-2-propenoic acid ethyl ester was placed in a flask in ice water. 12.67 g (0.275 mol) of methylhydrazine was added with stirring keeping the temperature below 40° C. After the addition, the flask was removed from the ice bath and left standing for 3 days at ambient temperature. The reaction mixture was treated with 250 ml of aqueous sodium bicarbonate, washed with water, filtered and dried in vacuo to give 16.1 g (30% yield) of a white solid, m.p. 119°-124° C.
Workup
- customthe temperature below 40° C
- additionAfter the addition
- customthe flask was removed from the ice bath
- waitleft
- additionThe reaction mixture was treated with 250 ml of aqueous sodium bicarbonate
- washwashed with water
- filtrationfiltered
- customdried in vacuo
Sources & evidence
- ORD record
- ord-27aabf811992490faed21fe88c5e027e
- Source dataset
- uspto-grants-1989_08
- Patent number
- US04855442
Reaction notes
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