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Carbon Disulfide → Benzyl (4-phenyl)dithiobenzoate

HRID 1926558
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HRID 1926558 반응식
[C:1]1([C:7]2[CH:12]=[CH:11][C:10]([Mg]Br)=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:15](=[S:17])=[S:16].[CH2:18](Br)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>O1CCCC1>[C:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:15]([S:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[S:16])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6348Carbon DisulfideHCID 7498Benzyl BromideHCID 178419618HCID 178419618, 화합물

생성물 1

HCID 59819145Benzyl (4-phenyl)dithiobenzoate수율 87%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

In 50 mL of dry tetrahydrofuran, 204 mL of (4-phenyl)phenyl magnesium bromide (a 0.5M tetrahydrofuran solution) was added, and the resulting mixture was stirred and then cooled to 0° C. While keeping 0° C., 7.77 g of carbon disulfide was added over 15 minutes, and the resulting mixture was stirred at 0° C. for 1 hour. Subsequently, 15.86 g of benzyl bromide was added over 15 minutes, and the resulting mixture was stirred at room temperature for 1 hour. After adding 300 mL of ice water, the organic layer was extracted with 500 mL of ethyl acetate. Furthermore, the organic layer was washed with 300 mL of brine and dried over anhydrous magnesium sulfate. The anhydrous magnesium sulfate was removed by filtration, and the residual solvent was then removed. The residue was purified on silica gel (ethyl acetate/hexane solvent) to obtain benzyl (4-phenyl)dithiobenzoate (28.4 g, yield: 87%) (exchange-chain transfer type RAFT agent).

후처리

  1. customWhile keeping 0° C.
  2. stirringthe resulting mixture was stirred at 0° C. for 1 hour
  3. stirringthe resulting mixture was stirred at room temperature for 1 hour
  4. extractionthe organic layer was extracted with 500 mL of ethyl acetate
  5. washFurthermore, the organic layer was washed with 300 mL of brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe anhydrous magnesium sulfate was removed by filtration
  8. customthe residual solvent was then removed
  9. customThe residue was purified on silica gel (ethyl acetate/hexane solvent)

출처 및 근거

ORD 기록
ord-047dd168e653488f89b31c8c6fa89d68
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08182975B2

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