Hydrazine → HCID 178507294, compound

HRID 2280407Notes

Reaction equation

HRID 2280407 reaction equation
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=O)[CH2:16][C:17]#[N:18])=[C:11]([F:20])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:21][NH2:22]>C(O)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[C:17]([NH2:18])[NH:22][N:21]=2)=[C:11]([F:20])[CH:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

4

Procedure

3-(4-(Benzyloxy)-2-fluorophenyl)-3-oxopropanenitrile (1.7 g, 6.3 mmol) was dissolved in ethanol (21 mL), and then hydrazine (0.22 mL, 6.9 mmol) was added. The reaction mixture was stirred at room temperature for about one hour, and the progress of the reaction was followed by thin-layer chromatography. If no progress had been made, the temperature was gradually increased until the reaction began proceeding. As soon as the reaction appeared complete by thin-layer chromatography, the crude material was concentrated in vacuo and purified by chromatography to provide the title compound 97% yield.

Workup

  1. temperaturethe temperature was gradually increased until the reaction
  2. concentrationthe crude material was concentrated in vacuo
  3. custompurified by chromatography

Sources & evidence

ORD record
ord-5a9919ce11f94c7db58bf063af9c0009
Source dataset
uspto-grants-2015_09
Patent number
US09139532B2

Reaction notes

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