Methylhydrazine → HCID 70584361, compound

HRID 1390804Notes

Reaction equation

HRID 1390804 reaction equation
[CH3:1][O:2][C:3]1[CH:36]=[C:35]([O:37][CH3:38])[CH:34]=[CH:33][C:4]=1[CH2:5][N:6]1[C:9](=[O:10])[C@H:8]([N:11]2C(=O)C3=CC=CC=C3C2=O)[C@@H:7]1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[CH:28]1[O:32][CH2:31][CH2:30][O:29]1.CNN>C(Cl)Cl>[NH2:11][C@H:8]1[C:9](=[O:10])[N:6]([CH2:5][C:4]2[CH:33]=[CH:34][C:35]([O:37][CH3:38])=[CH:36][C:3]=2[O:2][CH3:1])[C@H:7]1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[CH:28]1[O:32][CH2:31][CH2:30][O:29]1

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 70586021HCID 70586021, compound

Product 1

HCID 70584361HCID 70584361, compoundYield 107.3%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

The product from Example 2 (5.8 g) was dissolved in methylene chloride (40 ml) and filtered to remove a trace of insoluble solids (0.15 g). The filtrate was cooled with an ice bath and treated under a nitrogen atmosphere with methylhydrazine (0.85 g, 18.7 mmol). The reaction was stirred 2 days under nitrogen at room temperature and then filtered to remove a solid, which was washed with a small amount of methylene chloride. The filtrate ws evaporated in vacuo to give 4.65 g of the title product.

Workup

  1. filtrationfiltered
  2. customto remove a trace of insoluble solids (0.15 g)
  3. temperatureThe filtrate was cooled with an ice bath
  4. filtrationfiltered
  5. customto remove a solid, which
  6. washwas washed with a small amount of methylene chloride
  7. customThe filtrate ws evaporated in vacuo

Sources & evidence

ORD record
ord-9d39270297ef4590856025b3b651f47c
Source dataset
uspto-grants-1979_02
Patent number
US04140688

Reaction notes

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