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Benzyl mercaptan → (Benzylsulfanyl)(tributyl)stannane

HRID 1840528
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반응식

HRID 1840528 반응식
CCCCCCC=CCCC.[C:12]1([CH2:18][SH:19])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[CH2:20]([Sn:24](Cl)([CH2:29][CH2:30][CH2:31][CH3:32])[CH2:25][CH2:26][CH2:27][CH3:28])[CH2:21][CH2:22][CH3:23]>CN(C=O)C.CCCCC>[CH2:29]([Sn:24]([CH2:20][CH2:21][CH2:22][CH3:23])([CH2:25][CH2:26][CH2:27][CH3:28])[S:19][CH2:18][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[CH2:30][CH2:31][CH3:32]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7509Benzyl mercaptanHCID 15096Tributyltin ChlorideHCID 136496Undec-4-ene

생성물 1

HCID 12514237(Benzylsulfanyl)(tributyl)stannane수율 95%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8003Pentane용매

반응 조건

온도
0 °C

실험 절차

]undec-7-ene (DBU) is added dropwise at 20° C., under argon, to a solution of benzenemethanethiol (11.72 ml; 100.0 mmol) in anhydrous DMF (20.0 ml). After 0.5 hour at 20° C., the reaction mixture is cooled to 0° C. and tributyltin chloride is added dropwise. The mixture is allowed to warm to room temperature and stirring is continued for 5 hours. The reaction mixture is taken up in pentane (400 ml), washed with water (3×300 ml) and brine (100 ml), washed with sodium sulphate, filtered and then concentrated under reduced pressure. 39.0 g of tributyl[(phenylmethyl)thio]stannane are obtained in the form of a colourless oil, which is used without further purification in the following step.

후처리

  1. temperatureto warm to room temperature
  2. waitis continued for 5 hours
  3. washwashed with water (3×300 ml) and brine (100 ml)
  4. washwashed with sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7bbc2c1703044a6ba3458c2cbf9f1523
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06680329B2

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