Pyridine → HCID 12709388, 화합물

HRID 1265939노트

반응식

HRID 1265939 반응식
[OH:1][N:2]1[C:7]([CH3:9])([CH3:8])[CH2:6][CH:5](O)[CH2:4][C:3]1([CH3:12])[CH3:11].N(O[C:16]([CH3:19])([CH3:18])[CH3:17])=O.CC([O:24]NC1C=CC=CC=1)C=C.N1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1>>[O:24]1[C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][C:18]=2[CH:16]([CH2:19][O:1][N:2]2[C:7]([CH3:9])([CH3:8])[CH2:6][CH2:5][CH2:4][C:3]2([CH3:12])[CH3:11])[CH2:17]1

참가 물질

5

반응물 4

HCID 1049Pyridine2회HCID 53951,4-Dihydroxy-2,2,6,6-tetramethylpiperidineHCID 10906Tert-Butyl nitriteHCID 12032614HCID 12032614, 화합물

생성물 1

HCID 12709388HCID 12709388, 화합물수율 92.4%

실험 절차

The procedure of Example 1 is repeated using 3.0 g (19 mmol) of 1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine, 4.64 g (45 mmol) of tert-butyl nitrite, 11.45 mg (0.019 mmol) of (S,S)-(+)-N,N-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt(II) mmol) in 80 mL of pyridine and 6.27 g (38 mmol) of 2-(1-methylallyloxyaniline in 10 mL of pyridine. The crude product obtained is purified by vacuum flash chromatography (25% ethyl acetate/heptane) to give 5.31 g of a viscous liquid in 92.4% yield. The cis and trans isomers can be further separated by chromatography. The structures are confirmed by 1Hnmr analysis.

후처리

  1. customThe crude product obtained
  2. customis purified by vacuum flash chromatography (25% ethyl acetate/heptane)

출처 및 근거

ORD 기록
ord-01d3993abe7743659cf08847fc301361
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06547841B2

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