Water → HCID 178442570, 화합물

HRID 980780노트

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HRID 980780 반응식
[CH2:1]([C:9]1[S:13][C:12]2[S:14][C:15]([CH:17]=[O:18])=[CH:16][C:11]=2[CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH2:19]([CH:24]([CH2:27]O)[CH2:25][OH:26])[CH2:20][CH2:21][CH2:22][CH3:23].C1(C)C(S(O)(=O)=O)=CC=CC=1.O>C1(C)C=CC=CC=1>[CH2:1]([C:9]1[S:13][C:12]2[S:14][C:15]([C@H:17]3[O:26][CH2:25][C@H:24]([CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[CH2:27][O:18]3)=[CH:16][C:11]=2[CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 69252-Methylbenzenesulfonic acidHCID 1175092-Pentyl-1,3-propanediolHCID 202204675-n-Octylthieno[2,3-b]thiophene-2-carbaldehyde

생성물 1

HCID 178442570HCID 178442570, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

20.4 g of 5-n-octylthieno[2,3-b]thiophene-2-carbaldehyde (obtainable from 2-n-octylthieno[2,3-b]thiophene by Vilsmeyer formylation with phosphorus oxychloride/dimethylformamide) and 9.5 g of 2-n-pentylpropane-1,3-diol are dissolved in 150 ml of toluene, a pinch of toluenesulfonic acid is added, and the mixture is heated under a water separator until water is no longer separated off. The acid is washed out with sodium bicarbonate solution, the organic phase is dried over sodium sulfate, and the toluene is distilled off. The pure trans-2-(5-n-octylthieno[2,3-b]thien-2-yl)-5-n-pentyl-1,3-dioxane is obtained by repeated recrystallization from ethanol (17.5 g).

후처리

  1. temperaturethe mixture is heated under a water
  2. customis no longer separated off
  3. washThe acid is washed out with sodium bicarbonate solution
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. distillationthe toluene is distilled off

출처 및 근거

ORD 기록
ord-c0e5f1949c2648158bb7199aad31aae6
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04639328

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