Pyridine → HCID 12709388、化合物

HRID 1265939ノート

反応式

HRID 1265939 の反応式
[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

参加物

5

反応物 4

HCID 1049Pyridine2 回HCID 53951,4-Dihydroxy-2,2,6,6-tetramethylpiperidineHCID 10906Tert-Butyl nitriteHCID 12032614HCID 12032614、化合物

生成物 1

HCID 12709388HCID 12709388、化合物収率 92.4%

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-01d3993abe7743659cf08847fc301361
出典データセット
uspto-grants-2003_04
特許番号
US06547841B2

反応ノート

読み込み中…