Trichloroacetyl chloride → HCID 57098043、化合物

HRID 652986ノート

反応式

HRID 652986 の反応式
[CH2:1]([O:8][CH2:9][C:10]([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH2:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:31](Cl)(Cl)[C:32](Cl)=[O:33].P(Cl)(Cl)(Cl)=O>[Cu].[Zn].C(OCC)C>[CH2:1]([O:8][CH2:9][C:10]1([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH2:31][C:32](=[O:33])[CH2:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 6420Trichloroacetyl chlorideHCID 24813Phosphorus oxychlorideHCID 20196448HCID 20196448、化合物

生成物 1

HCID 57098043HCID 57098043、化合物

試薬・触媒・溶媒 2

HCID 10290809Zinc copper couple触媒HCID 3283Diethyl Ether溶媒

実験手順

A stirred mixture containing 7.18 g (18 mmol) of the compound prepared in (a) above, 75 ml of anhydrous diethyl ether and 1.4 g of zinc-copper couple was blanketed with nitrogen and treated dropwise at room temperature with a solution containing 3.63 g (20 mmol) of trichloroacetyl chloride and 3.06 g (20 mmol) of phosphorus oxychloride. After stirring the mixture at room temperature for 48 hours, the salts were filtered off and the filtrate concentrated in vacuo. The residue was then chromatographed on silica gel employing a mixture of petroleum ether and methyl-t-butyl ether in a ratio of 9:1 as the eluent to yield a yellow oil.

後処理

  1. additiontreated dropwise at room temperature with a solution
  2. filtrationthe salts were filtered off
  3. concentrationthe filtrate concentrated in vacuo
  4. customThe residue was then chromatographed on silica gel employing
  5. additiona mixture of petroleum ether and methyl-t-butyl ether in a ratio of 9:1 as the eluent
  6. customto yield a yellow oil

出典と根拠

ORDレコード
ord-fa953e530a6b4e9fa8d35264a3965288
出典データセット
uspto-grants-1987_06
特許番号
US04673672

反応ノート

読み込み中…