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Dimethylformamide → HCID 67298168, 화합물

HRID 1520303
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HRID 1520303 반응식
[N+:1]([C:4]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH3:16])=[CH:9][C:5]=1[C:6](O)=[O:7])([O-:3])=[O:2].C[N:18](C=O)C>O=S(Cl)Cl>[N+:1]([C:4]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH3:16])=[CH:9][C:5]=1[C:6]([NH2:18])=[O:7])([O-:3])=[O:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6228DimethylformamideHCID 127191782-Nitro-5-propoxybenzoic acid

생성물 1

HCID 67298168HCID 67298168, 화합물수율 85.2%

시약·촉매·용매 1

HCID 24386Thionyl Chloride용매

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온도
65 °C

실험 절차

A mixture of 2-nitro-5-propoxy-benzoic acid (1.97 g, 8.75 mmol) and DMF (0.1 mL) in SOCl2 (20 mL) was stirred at 65° C. for 2 h. After the reaction was completed, the mixture was cooled to room temperature. SOCl2 was removed in vacuo and the residue was dissolved in anhydrous CH2Cl2 (10 mL), which was added to NH3—H2O (28%) dropwise. After 1 h, the precipitate was collected and dried in vacuo to give 1.68 g of i-a as a yellow solid (85.2%). LCMS m/z=208.1 (M−16), 225.1 (M+1) (Method B) (retention time=1.88 min).

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

후처리

  1. temperaturethe mixture was cooled to room temperature
  2. customSOCl2 was removed in vacuo
  3. dissolutionthe residue was dissolved in anhydrous CH2Cl2 (10 mL)
  4. additionwhich was added to NH3—H2O (28%) dropwise
  5. waitAfter 1 h
  6. customthe precipitate was collected
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-6fa2de3290c544e681388b79ca95d6df
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073890B2

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