Water → 4-Carbethoxyphenyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthylmethyl ether

HRID 483717

반응식

HRID 483717 반응식
Br[CH2:2][C:3]1[CH:12]=[CH:11][C:10]2[C:9]([CH3:14])([CH3:13])[CH2:8][CH2:7][C:6]([CH3:16])([CH3:15])[C:5]=2[CH:4]=1.[OH:17][C:18]1[CH:28]=[CH:27][C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:13][C:9]1([CH3:14])[CH2:8][CH2:7][C:6]([CH3:16])([CH3:15])[C:5]2[CH:4]=[C:3]([CH2:2][O:17][C:18]3[CH:19]=[CH:20][C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:27][CH:28]=3)[CH:12]=[CH:11][C:10]1=2

참가 물질

6

반응물 4

HCID 962WaterHCID 8434EthylparabenHCID 11430Potassium CarbonateHCID 27355976-(Bromomethyl)-1,1,4,4-Tetramethyl-1,2,3,4-Tetrahydronaphthalene

생성물 1

HCID 148505914-Carbethoxyphenyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthylmethyl ether수율 50.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

10 g (36 mmol) of 2-bromomethyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene, 6 g (36 mmol) of ethyl 4-hydroxybenzoate and 7.2 g (52 mmol) of anhydrous potassium carbonate in 60 ml of dimethylformamide were refluxed for 5.25 h. The mixture was then poured into water and extracted several times with ether, and the organic phase was washed with water, dried over Na2SO4 and concentrated. Recrystallization from methanol resulted in 6.7 g of the title compound of melting point 109°-11° C.

후처리

  1. extractionextracted several times with ether
  2. washthe organic phase was washed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-728734cd98fd45dd97a4243fd8fb9546
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05225601

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