Toluene → HCID 86648189, 화합물

HRID 1047476노트

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HRID 1047476 반응식
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

참가 물질

4

반응물 3

HCID 1140TolueneHCID 6101p-Toluenesulfonic acidHCID 59608931HCID 59608931, 화합물

생성물 1

HCID 86648189HCID 86648189, 화합물

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-7abffe9df4d547b4a3e884409b53e4bb
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569532B2

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