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Triethylamine → 1-Monofluoro-2-decyl 4-octyloxybiphenyl-4'-carboxylate

HRID 1728521
ノート
印刷プレビュー

反応式

HRID 1728521 の反応式
[F:1][CH2:2][CH:3]([OH:12])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].C(N(CC)CC)C.[CH2:20]([O:28][C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][C:38]([C:41](Cl)=[O:42])=[CH:37][CH:36]=2)=[CH:31][CH:30]=1)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]>C(Cl)Cl.O>[CH2:20]([O:28][C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][C:38]([C:41]([O:12][CH:3]([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])[CH2:2][F:1])=[O:42])=[CH:37][CH:36]=2)=[CH:31][CH:30]=1)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 110784734-(4-Octyloxyphenyl)benzoyl chlorideHCID 146853301-Monofluoro-2-decanol

生成物 1

HCID 190139291-Monofluoro-2-decyl 4-octyloxybiphenyl-4'-carboxylate収率 58.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344
Dichloromethane
溶媒
2 回

実験手順

To a solution of optically active 1-monofluoro-2-decyl alcohol (0.1 g) and triethylamine (0.06 g) in methylene chloride (10 ml) was slowly added under ice cooling a solution of 4-n-octyloxybiphenyl-4'-carboxylic acid chloride (0.22 g) in methylene chloride (10 ml). The mixture was left to stand until it reached room temperature and stirred overnight. The mixture was poured in water and extracted with methylene chloride. The solution extracted layer was washed with dilute aqueous hydrochloric acid solution, water, 1N aqueous sodium carbonate solution and water, in this order, and dehydrated over anhydrous magnesium sulfate. After the solution was distilled under reduced pressure to remove the solvent, purification was made by silica-gel column chromatography to obtain the titled compound (0.16 g).

後処理

  1. waitThe mixture was left
  2. customreached room temperature
  3. extractionextracted with methylene chloride
  4. extractionThe solution extracted layer
  5. washwas washed with dilute aqueous hydrochloric acid solution, water, 1N aqueous sodium carbonate solution and water, in this order
  6. distillationAfter the solution was distilled under reduced pressure
  7. customto remove
  8. customthe solvent, purification

出典と根拠

ORDレコード
ord-c4023e5f2c2c4dde861b43a740c7f1df
出典データセット
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05328641

反応ノート

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