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Potassium Hydroxide → HCID 13302029、化合物

HRID 1709008
ノート
印刷プレビュー

反応式

HRID 1709008 の反応式
[S:1]1[CH2:6][CH2:5][CH2:4][S:3][C:2]1=[C:7]([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[CH:20]=1)[C:8]([O:10]CCCCCCCC)=[O:9].[OH-].[K+]>C(O)C.O>[S:1]1[CH2:6][CH2:5][CH2:4][S:3][C:2]1=[C:7]([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:26])([F:27])[F:28])[CH:20]=1)[C:8]([OH:10])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 13302038HCID 13302038、化合物

生成物 1

HCID 13302029HCID 13302029、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of n-octyl (1,3-dithian-2-ylidene)-(3-trifluoromethylphenyl)-acetate (15 g) in ethanol (375 ml), a 30% solution of potassium hydroxide in water (375 ml) is added. The mixture is refluxed for 2 hours. The solvents are removed in vacuo. Water (500 ml) and ether (500 ml) are added. The water solution is acidified to pH 4 with 5N sulphuric acid. The phases are separated and the water solution is extracted with ether (3×350 ml). The combined organic solutions are dried over magnesium sulphate and the solvent is evaporated in vacuo. The residue is triturated in petrol ether (b.p. 40°-65°) and dried in vacuo to constant weight to give (1,3-dithian-2-ylidene)-(3-trifluoromethylphenyl)-acetic acid, m.p. 165°-166° C.

後処理

  1. temperatureThe mixture is refluxed for 2 hours
  2. customThe solvents are removed in vacuo
  3. additionWater (500 ml) and ether (500 ml) are added
  4. customThe phases are separated
  5. extractionthe water solution is extracted with ether (3×350 ml)
  6. dry with materialThe combined organic solutions are dried over magnesium sulphate
  7. customthe solvent is evaporated in vacuo
  8. customThe residue is triturated in petrol ether (b.p. 40°-65°)
  9. customdried in vacuo to constant weight

出典と根拠

ORDレコード
ord-6959926cd203474b9710878c749fe859
出典データセット
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04946861

反応ノート

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