4-tert-Butylphenol → HCID 22759343, 화합물

HRID 329289노트

반응식

HRID 329289 반응식
[C:1]([CH:4]([CH2:16][CH2:17][CH2:18][CH:19]1[O:21][CH2:20]1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([O:13]CC)=[O:12])(=[O:3])[CH3:2].[C:22]([C:26]1[CH:31]=[CH:30][C:29]([OH:32])=[CH:28][CH:27]=1)([CH3:25])([CH3:24])[CH3:23].[OH-].[Na+]>O.O1CCCC1>[C:1]([CH:4]([CH2:16][CH2:17][CH2:18][CH:19]([OH:21])[CH2:20][O:32][C:29]1[CH:30]=[CH:31][C:26]([C:22]([CH3:25])([CH3:24])[CH3:23])=[CH:27][CH:28]=1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12])(=[O:3])[CH3:2]

참가 물질

6

반응물 3

HCID 73934-tert-ButylphenolHCID 14798Sodium HydroxideHCID 22759269HCID 22759269, 화합물

생성물 1

HCID 22759343HCID 22759343, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매2회

실험 절차

A mixture of ethyl 8-acetyl-12,13-epoxytridecanoate (14.9 g., 0.05 mole), 4-tert-butylphenol (11.2 g., 0.075 mole), sodium hydroxide (7.0 g., 0.175 mole), water (30 ml.) and tetrahydrofuran (200 ml.) is stirred 4 hours at 40°-45°, 17 hours at 25° and one hour on the steam bath letting the tetrahydrofuran slowly boil away. The residue is treated with water and extracted with ether. The aqueous solution is acidified with hydrochloric acid. The oily product is taken up in ether. The ether is evaporated and the residue treated with a solution of 16.8 g. sodium bicarbonate in 275 ml. of water. The resulting solution is extracted twice with ether to remove the excess weakly acidic phenol. The aqueous solution is acidified, the product taken up in ether, washed with water and dried over sodium sulfate. The ether is evaporated leaving 10.2 g. of the crude title compound as a yellow viscous oil.

후처리

  1. extractionextracted with ether
  2. customThe ether is evaporated
  3. additionthe residue treated with a solution of 16.8 g
  4. extractionThe resulting solution is extracted twice with ether
  5. customto remove the excess weakly acidic phenol
  6. washwashed with water
  7. dry with materialdried over sodium sulfate
  8. customThe ether is evaporated
  9. customleaving 10.2 g

출처 및 근거

ORD 기록
ord-624b5627838a4197af645ab138d02873
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04020177

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