Hydrochloric Acid → N'-methyl(tert-butoxy)carbohydrazide

HRID 1461879ノート

反応式

HRID 1461879 の反応式
[CH3:1][C:2]([CH3:20])([O:4][C:5]([NH:7][N:8](C(OCC1C=CC=CC=1)=O)[CH3:9])=[O:6])[CH3:3].Cl>CO.[Pd]>[CH3:1][C:2]([CH3:20])([O:4][C:5]([NH:7][NH:8][CH3:9])=[O:6])[CH3:3]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 110332501-Benzyl 2-tert-butyl 1-methylhydrazine-1,2-dicarboxylate

生成物 1

HCID 15671306N'-methyl(tert-butoxy)carbohydrazide収率 71.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of 1-[(1,1-dimethylethoxy)carbonyl]-2-[(phenylmethoxy)carbonyl]-2-methylhydrazine (15.0 g, 53. mmole) in 100 ml of methanol containing 4.9 ml of concentrated hydrochloric acid was hydrogenated at 1 atm in the presence of 3.0 g of 10% palladium-on-charcoal catalyst for 1 hour. The catalyst was filtered and the solvents were removed in vacuo. The residue was dissolved in water, the pH adjusted to 8.0 with sodium hydroxide and the mixture was extracted with ethyl acetate. The organic phase was dried over magnesium sulfate and evaporated to give 5.6 g of the title compound as a colorless solid, m.p. 50° C.

後処理

  1. filtrationThe catalyst was filtered
  2. customthe solvents were removed in vacuo
  3. dissolutionThe residue was dissolved in water
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic phase was dried over magnesium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-a0c5cdcdbb184738b2033ac1bae4d638
出典データセット
uspto-grants-1991_12
特許番号
US05077432

反応ノート

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