p-Toluenesulfonic acid → HCID 22590342, 화합물

HRID 23756

반응식

HRID 23756 반응식
[CH2:1]([O:4][C:5]1[C:9]([O:10][CH2:11][CH2:12][CH3:13])=[CH:8][S:7][CH:6]=1)CC.C(O)C(O)CC[CH2:18][CH2:19][OH:20].C1(C)C=CC(S(O)(=O)=O)=CC=1>>[O:10]1[CH:11]([CH2:12][CH2:13][CH2:18][CH2:19][OH:20])[CH2:1][O:4][C:5]2=[CH:6][S:7][CH:8]=[C:9]12

참가 물질

4

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 78231,2,6-HexanetriolHCID 114013973,4-Di-n-propoxythiophene

생성물 1

HCID 22590342HCID 22590342, 화합물

실험 절차

9.06 g (45.2 mmol) of 3,4-di-n-propoxythiophene, 30.3 g (226 mmol) of 1,2,6-hexanetriol and 0.09 g (0.5 mmol) of p-toluenesulphonic acid are heated to 150 to 165° C. (bath temperature) under N2 for 3 h. During this time, 5.8 g of distillate (substantially n-propanol) were collected. The cooled liquid was diluted with 50 ml of methylene chloride, washed to neutrality and to free it of hexanetriol with water and the organic phase was dried over Na2SO4. After filtering and evaporating the methylene chloride, the residue (6.73 g=74.8% of theory) was identified by 1H NMR spectroscopy (in CDCl3 against TMS) using δ=6.30 ppm (2H, thiophene H) and 2.85 ppm (1H, OH) as being substantially 4-(2,3-dihydrothieno[3,4-b][1,4]dioxin-2-yl)-1-butanol.

후처리

  1. distillationDuring this time, 5.8 g of distillate (substantially n-propanol) were collected
  2. additionThe cooled liquid was diluted with 50 ml of methylene chloride
  3. washwashed to neutrality
  4. dry with materialthe organic phase was dried over Na2SO4
  5. filtrationAfter filtering
  6. customevaporating the methylene chloride

출처 및 근거

ORD 기록
ord-d92287d6b2ae41aa84fbe9104e260357
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852831B2

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