Triethylamine → N-tert-butyl-N-ethoxalyl-2-nitroaniline

HRID 358952노트

반응식

HRID 358952 반응식
[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=1[NH:6][C:7]([CH3:10])([CH3:9])[CH3:8])([O-:3])=[O:2].C(N(CC)CC)C.[C:22](Cl)([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[O:23]>O1CCCC1>[C:7]([N:6]([C:22]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[O:23])[C:5]1[CH:11]=[CH:12][CH:13]=[CH:14][C:4]=1[N+:1]([O-:3])=[O:2])([CH3:10])([CH3:8])[CH3:9]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 10797892N-tert-Butyl-2-nitroaniline

생성물 1

HCID 20065638N-tert-butyl-N-ethoxalyl-2-nitroaniline

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a stirred solution of 2-nitro-N-tert-butylaniline (37 g) and triethylamine (35 ml) in tetrahydrofuran (400 ml) was added dropwise a solution of ethoxalyl chloride (25 ml) in tetrahydrofuran (50 ml). The mixture was then brought to reflux temperature for 8 h. The solvent was removed by evaporation, and the residue was partitioned between ether (300 ml) and water (500 ml). The organic phase was washed twice with water, dried over Na2SO4 and evaporated. This left the title compound as light yellow crystals, m.p. 73°-74° C.

후처리

  1. temperatureto reflux temperature for 8 h
  2. customThe solvent was removed by evaporation
  3. customthe residue was partitioned between ether (300 ml) and water (500 ml)
  4. washThe organic phase was washed twice with water
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. waitThis left the title compound as light yellow crystals, m.p. 73°-74° C.

출처 및 근거

ORD 기록
ord-231e8e5054254f97a84ddcc59e54f853
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04999353

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