Trichloroacetyl chloride → HCID 57098043, 화합물

HRID 652986노트

반응식

HRID 652986 반응식
[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

참가 물질

6

반응물 3

HCID 6420Trichloroacetyl chlorideHCID 24813Phosphorus oxychlorideHCID 20196448HCID 20196448, 화합물

생성물 1

HCID 57098043HCID 57098043, 화합물

시약·촉매·용매 2

HCID 10290809Zinc copper couple촉매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fa953e530a6b4e9fa8d35264a3965288
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673672

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