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Benzoic Acid → Benzyl dithiobenzoate

HRID 990257
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인쇄 미리보기

반응식

HRID 990257 반응식
[C:1](O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:10]([SH:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:19]>C1(C)C=CC=CC=1>[C:1]([S:17][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)(=[S:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 243Benzoic AcidHCID 7509Benzyl mercaptanHCID 14817Phosphorus sulfide (P2S5)

생성물 1

HCID 11459208Benzyl dithiobenzoate수율 91%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of benzoic acid (1.22 g), benzyl mercaptan (1.24 g) and phosphorus pentasulfide (4.44 g) in toluene (40 ml) was refluxed for 10 h. A dark red color was developed immediately after heating. After the reaction was complete (as monitored by GC-MS), it was cooled to room temperature and purified by column chromatography packed with.neutral alumina, eluting with benzene. Removal of the solvent by distillation gave the single compound, benzyl dithiobenzoate (2.22 g, 91%). It was further characterized by 1H and 13C-NMR.

후처리

  1. temperaturewas refluxed for 10 h
  2. temperatureafter heating
  3. custompurified by column chromatography
  4. washeluting with benzene
  5. customRemoval of the solvent
  6. distillationby distillation

출처 및 근거

ORD 기록
ord-26115d13a3024401b498fe143ffdb59f
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06458968B2

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