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Octanoyl chloride → HCID 58534629, 화합물

HRID 1466968
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HRID 1466968 반응식
[SH:1][CH2:2][CH2:3][CH2:4][Si:5]([CH3:10])([CH3:9])[O:6][CH2:7][CH3:8].C(N(CC)CC)C.[C:18](Cl)(=[O:26])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]>C1CCCCC1>[C:18]([S:1][CH2:2][CH2:3][CH2:4][Si:5]([O:6][CH2:7][CH3:8])([CH3:10])[CH3:9])(=[O:26])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]
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참가 물질

5

반응물 3

HCID 8124Octanoyl chlorideHCID 8471TriethylamineHCID 222272273-[Ethoxy(dimethyl)silyl]propane-1-thiol

생성물 1

HCID 58534629HCID 58534629, 화합물수율 78%

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

Added dropwise at 5° C., under argon, to 3-mercaptopropyldimethylethoxysilane (34.0 g, 0.191 mol) in solution in triethylamine (19.2 g, 0.191 mol) and cyclohexane (400 ml) is octanoyl chloride (31.0 g, 0.191 mol) over 15 minutes at 8° C. The reaction medium is stirred for 15 hours at ambient temperature. The precipitate of triethylamine hydrochloride Et3N.HCl is filtered. The mixture obtained is purified by flash chromatography (eluent: petroleum ether, 500-600 ml). After evaporating the solvents under reduced pressure at 24° C., the S-octanoylmercaptopropylethoxydimethylsilane E with CAS number [1024594-66-8] (45.0 g, 0.148 mol) is obtained in the form of a colourless liquid with a yield of 78%.

후처리

  1. customover 15 minutes
  2. customat 8° C
  3. filtrationThe precipitate of triethylamine hydrochloride Et3N.HCl is filtered
  4. customThe mixture obtained
  5. customis purified by flash chromatography (eluent: petroleum ether, 500-600 ml)
  6. customAfter evaporating the solvents under reduced pressure at 24° C.

출처 및 근거

ORD 기록
ord-6051b65e13f149e1896952798bcf0927
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09000092B2

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