Dimethylformamide → 3,5-Diethyl-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene

HRID 1280243노트

반응식

HRID 1280243 반응식
[CH2:1]([C:3]1[CH:4]=[C:5]([OH:25])[CH:6]=[C:7]([CH2:23][CH3:24])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][CH:16]([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[CH3:2].[Cl:26][C:27]([Cl:31])=[CH:28][CH2:29]Cl.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[CH2:23]([C:7]1[CH:6]=[C:5]([O:25][CH2:29][CH:28]=[C:27]([Cl:31])[Cl:26])[CH:4]=[C:3]([CH2:1][CH3:2])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][CH:16]([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[CH3:24]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 173781,1,3-TrichloropropeneHCID 184295323,5-Diethyl-4-(4-(2,2-diethoxyethoxy)butyloxy)phenol

생성물 1

HCID 184299913,5-Diethyl-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene수율 97.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Then, 19.9 g of 3,5-diethyl-4-(4-(2,2-diethoxyethoxy)butyloxy)phenol, 9.20 g of 1,1,3-trichloro-1-propene, 9.15 g of potassium carbonate, and 200 ml of N,N-dimethylformamide were placed in a reaction vessel. After stirring at room temperature for 24 hours, the reaction mixture was poured into water, and extracted twice with diethyl ether. The diethyl ether layers were combined, washed with water, dried over anhydrous magnesium, and concentrated to give a residue. This residue was subjected to silica gel chromatography, which afforded 25.4 g (yield, 91%) of 3,5-diethyl-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene, nD26.0 1.4991.

후처리

  1. extractionextracted twice with diethyl ether
  2. washwashed with water
  3. dry with materialdried over anhydrous magnesium
  4. concentrationconcentrated
  5. customto give a residue

출처 및 근거

ORD 기록
ord-2b3b6abd53b548bb80c0563a24aa0c89
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06448444B1

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