1,3-Butadiene → HCID 68771799、化合物

HRID 1172319ノート

反応式

HRID 1172319 の反応式
[CH2:1]=[CH:2][CH:3]=[CH2:4].[Cl:5][C:6]1[CH:16]=[CH:15][CH:14]=[CH:13][C:7]=1[CH:8]=[CH:9][N+:10]([O-:12])=[O:11]>C1(C)C=CC=CC=1>[Cl:5][C:6]1[CH:16]=[CH:15][CH:14]=[CH:13][C:7]=1[C@H:8]1[C@H:9]([N+:10]([O-:12])=[O:11])[CH2:4][CH:3]=[CH:2][CH2:1]1

参加物

4

反応条件

温度
110 °C

実験手順

A 10 mL solution of 1:1 1,3-butadiene and toluene stored at −20° C. and 2-chloro-β-nitrostyrene (2.0 g, 11 mmol) were added to a pressure tube and sealed. The solution was heated to 110° C. and stirred for three days. The reaction mixture was cooled to room temperature, concentrated, and the residue was crystallized from hexanes to give the title compound. 1H NMR (300 MHz, CDCl3) δ ppm 7.35-7.38 (m, 1H), 7.15-7.29 (m, 3H), 5.71-5.84 (m, 2H), 5.09-5.16 (m, 1H), 4.04-4.13 (m, 1H), 2.76-2.84 (m, 2H), 2.54-2.60 (m, 1H), 2.19-2.28 (m, 1H).

後処理

  1. customstored at −20° C.
  2. customsealed
  3. temperatureThe reaction mixture was cooled to room temperature
  4. concentrationconcentrated
  5. customthe residue was crystallized from hexanes

出典と根拠

ORDレコード
ord-3ab06f09a1864851a7c1f80cc1369f9f
出典データセット
uspto-grants-2010_11
特許番号
US07834012B2

反応ノート

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