2-Methoxyaniline → 2-Methoxycyclohexan-1-amine

HRID 1178932노트

반응식

HRID 1178932 반응식
[CH3:1][O:2][C:3]1[C:4]([NH2:9])=[CH:5][CH:6]=[CH:7][CH:8]=1>CC(O)=O.[Rh]>[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]1[NH2:9]

참가 물질

4

반응물 1

HCID 70002-Methoxyaniline

생성물 1

HCID 222508792-Methoxycyclohexan-1-amine수율 22.7%

시약·촉매·용매 2

HCID 23948Rhodium촉매HCID 176Acetic Acid용매

실험 절차

Shake a mixture of o-anisidine (5.0 g, 41 mmol) and rhodium on carbon (5% Rh; 5.0 g) in AcOH (65 mL) under H2 (60 psig) at 60° C. for 6 h. Filter the reaction mixture and rotary evaporate the filtrate (75° C.). Dissolve this material in CHCl3 (100 mL) and basify with satd aq NaHCO3 (50 mL). Dry the organic layer (Na2SO4) and rotary evaporate (40° C.) to yield 1.20 g of 2-methoxy-cyclohexylamine as a yellow oil.

후처리

  1. filtrationFilter the reaction mixture
  2. customrotary evaporate the filtrate (75° C.)
  3. dissolutionDissolve this material in CHCl3 (100 mL)
  4. dry with materialDry the organic layer (Na2SO4)
  5. customrotary evaporate (40° C.)

출처 및 근거

ORD 기록
ord-ce168f97f6b842cbad625ffa2bb369ba
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07276516B2

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