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4-Nitrobenzoic Acid → STK331703

HRID 990260
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HRID 990260 반응식
[N+:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8](O)=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH2:13]([SH:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>C1(C)C=CC=CC=1>[CH2:13]([S:20][C:8](=[S:22])[C:7]1[CH:11]=[CH:12][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 61084-Nitrobenzoic AcidHCID 7509Benzyl mercaptanHCID 14817Phosphorus sulfide (P2S5)

생성물 1

HCID 11415045STK331703수율 51.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 4-nitrobenzoic acid (1.67 g), benzyl mercaptan (1.24 g) and phosphorus pentasulfide (4.44 g) in toluene (40 ml) was refluxed for 20 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 a column chromatography packed with neutral alumina, eluting with benzene. Removal of the solvent by distillation gave the single compound, benzyl-4-nitrodithiobenzoate (1.48 g, 51%). It was further characterized by 1H and 13C-NMR.

후처리

  1. temperaturewas refluxed for 20 h
  2. temperatureafter heating
  3. custompurified by a column chromatography
  4. washeluting with benzene
  5. customRemoval of the solvent
  6. distillationby distillation

출처 및 근거

ORD 기록
ord-740fbc89090b4a61b9873d3853350b73
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06458968B2

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