Toluene → HCID 86648189、化合物

HRID 1047476ノート

反応式

HRID 1047476 の反応式
CO[CH:3]1[C:11]2[C:6](=[C:7]([CH2:14][CH2:15][C:16]3(O)[CH2:24][C:23]4[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=4)[CH2:17]3)[C:8]([CH3:13])=[C:9]([CH3:12])[CH:10]=2)[CH2:5][CH:4]1[CH3:26].C1(C)C=CC=CC=1.CC1C=CC(S(O)(=O)=O)=CC=1>>[CH2:24]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[C:16]1[CH2:15][CH2:14][C:7]1[C:8]([CH3:13])=[C:9]([CH3:12])[CH:10]=[C:11]2[C:6]=1[CH2:5][C:4]([CH3:26])=[CH:3]2

参加物

4

反応物 3

HCID 1140TolueneHCID 6101p-Toluenesulfonic acidHCID 59608931HCID 59608931、化合物

生成物 1

HCID 86648189HCID 86648189、化合物

実験手順

To a hot (110° C.) solution of 6.0 g (18.61 mmol) of 2-[2-(1-methoxy-2,5,6-trimethyl-2,3-dihydro-1H-inden-4-yl)ethyl]indan-2-ol in 130 ml of toluene 0.708 g (3.72 mmol) of TsOH*H2O was added. This mixture was refluxed with a Dean-Stark trap for 30 min, and then passed through short column with Silica Gel 60 (40-63 um, d 80 mm, l 60 mm). The column was additionally washed with 300 ml of toluene. The combined elute was evaporated to dryness. The product was isolated by flash chromatography using a short column with Silica Gel 60 (40-63 um, d 60 mm, l 70 mm; eluent: hexanes/ether=50/1). Yield 4.58 g (82%).

後処理

  1. temperatureThis mixture was refluxed with a Dean-Stark trap for 30 min
  2. washThe column was additionally washed with 300 ml of toluene
  3. washThe combined elute
  4. customwas evaporated to dryness
  5. customThe product was isolated by flash chromatography

出典と根拠

ORDレコード
ord-7abffe9df4d547b4a3e884409b53e4bb
出典データセット
uspto-grants-2013_10
特許番号
US08569532B2

反応ノート

読み込み中…