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Methyl 3,5-dinitro-2-((phenylmethyl)thio)benzoate → HCID 19987327, 화합물

HRID 2106951
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HRID 2106951 반응식
[CH3:1][O:2][C:3](=[O:24])[C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[CH:7]=[C:6]([N+:13]([O-])=O)[C:5]=1[S:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>O1CCCC1.[Ni]>[CH3:1][O:2][C:3](=[O:24])[C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[C:6]([NH2:13])[C:5]=1[S:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 2755032Methyl 3,5-dinitro-2-((phenylmethyl)thio)benzoate

생성물 1

HCID 19987327HCID 19987327, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 8028Tetrahydrofuran용매

실험 절차

The 2-benzylthio-3,5-dinitrobenzoic acid methyl ester obtained in the previous stage (see Example 1.14), which is still damp, is dissolved in 2 l of tetrahydrofuran and hydrogenated at from 30° to 35° C. with the addition of 3×40 g of Raney nickel. The catalyst is then removed by filtration, the filtrate is concentrated and the residue is taken up in ethyl acetate. After drying over magnesium sulfate and treating with activated carbon and fuller's earth, the filtrate is concentrated and the product is caused to crystallise by the addition of diethyl ether.

후처리

  1. customThe catalyst is then removed by filtration
  2. concentrationthe filtrate is concentrated
  3. dry with materialAfter drying over magnesium sulfate
  4. additiontreating with activated carbon and fuller's earth
  5. concentrationthe filtrate is concentrated
  6. customto crystallise by the addition of diethyl ether

출처 및 근거

ORD 기록
ord-dad2980fcd7a49b390cea03061b49e6b
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04931581

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