Water → HCID 178442570、化合物

HRID 980780ノート

反応式

HRID 980780 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 178442570HCID 178442570、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c0e5f1949c2648158bb7199aad31aae6
出典データセット
uspto-grants-1987_01
特許番号
US04639328

反応ノート

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