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2,6-Di-tert-butyl-4-mercaptophenol → HCID 14011801, 화합물

HRID 986295
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HRID 986295 반응식
[CH3:1][C:2]([C:5]1[CH:10]=[C:9]([SH:11])[CH:8]=[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:6]=1[OH:16])([CH3:4])[CH3:3].[O-][CH2:18]C.[Na+].[Na].Cl[CH2:23][CH2:24][S:25]([CH2:27][C:28]([O:30][CH3:31])=[O:29])=[O:26]>C(O)C.O>[CH3:4][C:2]([C:5]1[CH:10]=[C:9]([S:11][CH2:23][CH2:24][S:25]([CH2:27][C:28]([O:30][CH2:31][CH3:18])=[O:29])=[O:26])[CH:8]=[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:6]=1[OH:16])([CH3:1])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 703702,6-Di-tert-butyl-4-mercaptophenolHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 20133529HCID 20133529, 화합물

생성물 1

HCID 14011801HCID 14011801, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매2회
HCID 962
Water
용매

실험 절차

2,6-bis(1,1-Dimethylethyl)-4-mercaptophenol (2.97 g, 0.0125 mole) was added to sodium ethoxide, freshly prepared from sodium (0.29 g, 0.0125 mole) in ethyl alcohol (75 ml), and stirred for 1.5 hours. A solution of the title compound of Example 11 (2.3 g, 0.0125 mole) in ethyl alcohol (50 ml) was added dropwise over one hour and the resulting solution stirred for 20 hours at room temperature. Water (100 ml) was added and the ethyl alcohol removed using a rotary evaporator. The aqueous residue was extracted with ethyl acetate (2×100 ml). The combined organic extracts were dried over sodium sulfate, filtered, concentrated and the product purified by chromatography on silica. The yellow solid was recrystallized from ethyl acetate/hexane to give 1.1 g, m.p. ca. 110° C.

후처리

  1. stirringthe resulting solution stirred for 20 hours at room temperature
  2. customthe ethyl alcohol removed
  3. customa rotary evaporator
  4. extractionThe aqueous residue was extracted with ethyl acetate (2×100 ml)
  5. dry with materialThe combined organic extracts were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customthe product purified by chromatography on silica
  9. customThe yellow solid was recrystallized from ethyl acetate/hexane
  10. customto give 1.1 g, m.p. ca. 110° C.

출처 및 근거

ORD 기록
ord-c9e4d7d7aab34b2d883c7da385ca2841
출처 데이터셋
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04711903

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