Ammonium formate → 4-[2-(Oxan-2-yloxy)ethoxy]aniline

HRID 450512노트

반응식

HRID 450512 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12][O:13][CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][O:15]2)=[CH:6][CH:5]=1)([O-])=O.C([O-])=O.[NH4+]>CCO.[Pd]>[O:15]1[CH2:16][CH2:17][CH2:18][CH2:19][CH:14]1[O:13][CH2:12][CH2:11][O:10][C:7]1[CH:6]=[CH:5][C:4]([NH2:1])=[CH:9][CH:8]=1

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 108908362-[2-(4-Nitrophenoxy)ethoxy]oxane2회

생성물 1

HCID 110209174-[2-(Oxan-2-yloxy)ethoxy]aniline

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

반응 조건

온도
40 °C

실험 절차

To a solution of 2-({2-[(4-nitrophenyl)oxy]ethyl}oxy)tetrahydro-2H-pyran (Intermediate 17) (1.33 g, 5 mmol) in EtOH (50 mL) was added Pd/C (catalytic amount) and ammonium formiate (0.9 g, 10 eq). The reaction was stirred to 40° C. for 2 hours. After filtration on celite, the solvent was evaporated and the residue was poured in water, extracted with ether and dried over sodium sulphate and evaporated. The title compound was obtained as a dark oil (0.8 g, 68%). LC/MS: m/z 238 (M+H)+, Rt: 2.38 min.

후처리

  1. filtrationAfter filtration on celite
  2. customthe solvent was evaporated
  3. additionthe residue was poured in water
  4. extractionextracted with ether
  5. dry with materialdried over sodium sulphate
  6. customevaporated

출처 및 근거

ORD 기록
ord-deae8ce8f9d345edadeae3956c2458e5
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486977B2

반응 노트

불러오는 중…