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Thionyl Chloride → HCID 53773575、化合物

HRID 1612590
ノート
印刷プレビュー

反応式

HRID 1612590 の反応式
[CH2:1]([O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16](O)=[O:17])=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH:9]=[CH2:10].S(Cl)([Cl:23])=O>C1(C)C=CC=CC=1>[CH:1]([O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([Cl:23])=[O:17])=[CH:14][CH:13]=1)=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 148765254-(9-Decen-1-yloxy)benzoic acid

生成物 1

HCID 53773575HCID 53773575、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To 2.8 g of p-(9-decenyloxy)benzoic acid prepared in the same manner as in 9.(2) in Example 9 added was toluene, and the resulting mixture was cooled in an ice bath. 5.0 g of thionyl chloride was then added dropwise to the toluene solution. Reaction was then carried out for 7 hours at 80° C. After conclusion of the reaction, the reaction solution was concentrated under reduced pressure, to obtain crude p-decenyloxybenzoyl chloride. 1.6 g of the hydroxy compound obtained in 17.(1) and 3.3 g of pyridine were dissolved in toluene, and the resulting toluene solution was cooled in an ice bath. A toluene solution containing the above crude p-decenyloxybenzoyl chloride was added dropwise into the toluene solution. Subsequently, reaction was carried out for 5 hours at 50° C. After conclusion of the reaction, the reaction solution was washed with water and dried over magnesium sulfate, and the solvent was distilled out under reduced pressure. The residue was purified by column chromatography, to obtain 2.0 g of the objective alkene compound. (Yield: 69%)

後処理

  1. additionadded
  2. temperaturethe resulting mixture was cooled in an ice bath
  3. customReaction
  4. customAfter conclusion of the reaction
  5. concentrationthe reaction solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-e0135dd47e8d4a1599b38862a642e93c
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05190686

反応ノート

読み込み中…

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