Methylhydrazine → HCID 178481943, compound

HRID 1722461Notes

Reaction equation

HRID 1722461 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

  1. customthe temperature below 40° C
  2. additionAfter the addition
  3. customthe flask was removed from the ice bath
  4. waitleft
  5. additionThe reaction mixture was treated with 250 ml of aqueous sodium bicarbonate
  6. washwashed with water
  7. filtrationfiltered
  8. customdried in vacuo

Sources & evidence

ORD record
ord-27aabf811992490faed21fe88c5e027e
Source dataset
uspto-grants-1989_08
Patent number
US04855442

Reaction notes

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