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Water → HCID 89501539, 화합물

HRID 590540
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인쇄 미리보기

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HRID 590540 반응식
Cl.[CH3:2][Si:3]1([CH3:9])[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.C(N(CC)CC)C.[F:17][C:18]1[CH:19]=[C:20]([N+:25]([O-:27])=[O:26])[CH:21]=[CH:22][C:23]=1F.O>C(OC(=O)C)C>[F:17][C:18]1[CH:19]=[C:20]([N+:25]([O-:27])=[O:26])[CH:21]=[CH:22][C:23]=1[N:6]1[CH2:7][CH2:8][Si:3]([CH3:9])([CH3:2])[CH2:4][CH2:5]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 1230531,2-Difluoro-4-nitrobenzeneHCID 672158374,4-dimethyl-1,4-azasilinane hydrochloride

생성물 1

HCID 89501539HCID 89501539, 화합물수율 69.8%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
25 °C

실험 절차

To a solution of 4 (500 mg, 3.85 mmol) in ethylacetate, triethylamine (973 mg, 9.63 mmol) is added and stirred at 25° C. for 10 min. The reaction mixture is cooled to 0° C. and 3,4-difluoronitrobenzene (612 mg, 3.85 mmol) is added dropwise and allowed to stir at 25° C. for 6 h. Water is then added and the organic layer is separated. The aqueous layer is extracted with EtOAc and the solvent is removed. The product is purified by column chromatography using hexanes-EtOAc mixtures to obtain the product as a crystalline yellow solid 9 (721 mg) in 70% isolated yield.

후처리

  1. temperatureThe reaction mixture is cooled to 0° C.
  2. stirringto stir at 25° C. for 6 h
  3. customthe organic layer is separated
  4. extractionThe aqueous layer is extracted with EtOAc
  5. customthe solvent is removed
  6. customThe product is purified by column chromatography

출처 및 근거

ORD 기록
ord-1e2f53a0aac94e0a8a660d88714bea0e
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09233989B2

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