Potassium Carbonate → tert-Butyl (2-((5-methoxy-2-nitrophenyl)amino)ethyl)carbamate

HRID 1914920

반응식

HRID 1914920 반응식
C([O-])([O-])=O.[K+].[K+].[CH3:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[C:11](F)[CH:10]=1.[C:19]([NH:26][CH2:27][CH2:28][NH2:29])([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20]>CS(C)=O>[C:22]([O:21][C:19](=[O:20])[NH:26][CH2:27][CH2:28][NH:29][C:11]1[CH:10]=[C:9]([O:8][CH3:7])[CH:14]=[CH:13][C:12]=1[N+:15]([O-:17])=[O:16])([CH3:25])([CH3:23])[CH3:24]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 187201N-BOC-ethylenediamineHCID 5656543-Fluoro-4-nitroanisole

생성물 1

HCID 59345555tert-Butyl (2-((5-methoxy-2-nitrophenyl)amino)ethyl)carbamate수율 104%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
60 °C

실험 절차

A 2 L flask equipped with a stir bar was charged with DMSO (800 mL), K2CO3 (161 g, 1.6 mol) and 4-methoxy-2-fluoro-1-nitrobenzene (100 g, 0.58 mol). Mono-N-Boc-1,2-diaminoethane (94 g, 0.55 mol) was added to the reaction mixture and stirred for 12 h at 60° C. The reaction mixture was triturated with ice cold water (1.2 L) and the resulting yellow precipitate was collected by vacuum filtration. The precipitate was washed several times with water (5×1 L) and dried on a high vacuum for 48 h to give the desired product as a bright yellow solid (178 g, 98%.)

후처리

  1. customA 2 L flask equipped with a stir bar
  2. customThe reaction mixture was triturated with ice cold water (1.2 L)
  3. filtrationthe resulting yellow precipitate was collected by vacuum filtration
  4. washThe precipitate was washed several times with water (5×1 L)
  5. customdried on a high vacuum for 48 h

출처 및 근거

ORD 기록
ord-c416f85f63e34c768e0fc40e299a8a2e
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614243B2

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