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Hydrochloric Acid → HCID 19757561, 화합물

HRID 1587263
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HRID 1587263 반응식
C1(C)C=CC(S(O[CH2:11][CH2:12][CH2:13][Si:14]([CH2:17][CH2:18][CH2:19][CH3:20])([CH3:16])[CH3:15])(=O)=O)=CC=1.[C:22]1([CH:29]=[CH:28][C:26]([OH:27])=[CH:25][CH:24]=1)[OH:23].[OH-].[K+].Cl>O.C(O)C.CO>[CH2:17]([Si:14]([CH3:16])([CH3:15])[CH2:13][CH2:12][CH2:11][O:23][C:22]1[CH:29]=[CH:28][C:26]([OH:27])=[CH:25][CH:24]=1)[CH2:18][CH2:19][CH3:20]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 785HydroquinoneHCID 14797Potassium HydroxideHCID 19757560HCID 19757560, 화합물

생성물 1

HCID 19757561HCID 19757561, 화합물수율 50.6%

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 887
Methanol
용매
HCID 962Water용매

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온도
65 °C

실험 절차

The above-obtained 3-(butyldimethylsilyl)propyl p-toluenesulfonate was added dropwise in 45 min. to a mixture of 2.32 g (21.1 mM) of hydroquinone, 1.13 g (17.1 mM) of 85 %-potassium hydroxide, 6 ml of methanol and 30 ml of ethanol under stirring at 65° C., followed by stirring for 0.5 hour and further stirring for 6 hour at 80° C. After the reaction, the reaction mixture was poured into cold water, acidified with hydrochloric acid (pH≈2) and extracted with ethyl acetate, followed by washing with water and drying with anhydrous magnesium sulfate. The magnesium sulfate in the resultant mixture was filtered off and the filtrate was condensed into a solid, followed by purification by silica gel column chromatography (eluent: toluene) to obtain 2.05 g of 4-[3-(butyldimethylsilyl)propoxy]phenol (Yield: 50.6 %).

후처리

  1. stirringby stirring for 0.5 hour
  2. stirringfurther stirring for 6 hour at 80° C
  3. customAfter the reaction
  4. extractionextracted with ethyl acetate
  5. washby washing with water
  6. dry with materialdrying with anhydrous magnesium sulfate
  7. filtrationThe magnesium sulfate in the resultant mixture was filtered off
  8. customcondensed into a solid
  9. customfollowed by purification by silica gel column chromatography (eluent: toluene)

출처 및 근거

ORD 기록
ord-7fb995eaa5dd49e78960a2ebbc3b68d0
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05217645

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