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

HRID 1461879노트

반응식

HRID 1461879 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a0c5cdcdbb184738b2033ac1bae4d638
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05077432

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