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Hydrochloric Acid → HCID 19757560, 화합물

HRID 1587262
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HRID 1587262 반응식
[CH2:1]([Si:5]([CH3:11])([CH3:10])[CH2:6][CH2:7][CH2:8][OH:9])[CH2:2][CH2:3][CH3:4].N1C=CC=CC=1.[C:18]1([CH3:28])[CH:23]=[CH:22][C:21]([S:24](Cl)(=[O:26])=[O:25])=[CH:20][CH:19]=1.Cl>O>[C:18]1([CH3:28])[CH:23]=[CH:22][C:21]([S:24]([O:9][CH2:8][CH2:7][CH2:6][Si:5]([CH2:1][CH2:2][CH2:3][CH3:4])([CH3:10])[CH3:11])(=[O:26])=[O:25])=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 73974-Toluenesulfonyl chlorideHCID 197575723-[Butyl(dimethyl)silyl]propan-1-ol

생성물 1

HCID 19757560HCID 19757560, 화합물수율 81.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

5.0 g (28.68 mM) of butyldimethyl-3-hydroxypropylsilane was added 50 ml of pyridine, followed by stirring. To the mixture, 5.4 g (28.32 mM) of p-toluenesulfonyl chloride was added under cooling on an ice bath, followed by stirring for 0.5 hour and further stirring for 4 hours at room temperature. After the reaction, the reaction mixture was poured into 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 to obtain 3-(butyldimethylsilyl)propyl p-toluenesulfonate (Yield: 81.7 %).

후처리

  1. temperatureunder cooling on an ice bath
  2. stirringby stirring for 0.5 hour
  3. stirringfurther stirring for 4 hours at room temperature
  4. customAfter the reaction
  5. extractionextracted with ethyl acetate
  6. washby washing with water
  7. dry with materialdrying with anhydrous magnesium sulfate
  8. filtrationThe magnesium sulfate in the resultant mixture was filtered off
  9. customcondensed into a solid

출처 및 근거

ORD 기록
ord-ea5a4a9aa6c842c6a3bf55b4d6557101
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05217645

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