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Formic Acid → HCID 22712342, 화합물

HRID 394575
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HRID 394575 반응식
C=O.C(O)=O.[Br:6][C:7]1[CH:13]=[CH:12][C:10](N)=[C:9](C)[C:8]=1[N+:15]([O-:17])=[O:16].[CH3:18][N:19]([CH:21]=O)[CH3:20]>>[CH3:18][N:19]([CH3:20])[C:21]1[CH:12]=[CH:13][C:7]([Br:6])=[C:8]([N+:15]([O-:17])=[O:16])[C:9]=1[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 284Formic AcidHCID 712FormaldehydeHCID 6228Dimethylformamide2회HCID 227123394-Bromo-2-methyl-3-nitroaniline

생성물 1

HCID 22712342HCID 22712342, 화합물

실험 절차

5.8 g of paraformaldehyde and 15 ml of formic acid are dissolved in 15 ml of DMF and heated to 90° C.-100° C. A solution of 18 g of 4-bromo-2-methyl-3-nitroaniline in 15 ml of DMF is added dropwise within 10 minutes. After 2 hours, the mixture is added to about 600 ml of ice water and the aqueous phase is extracted with 300 ml of ether. The organic phase is washed with Na2CO3 (1M), filtered and evaporated down. The product is purified by chromatography (silica gel, eluant: petroleum ether/ethyl acetate (40/60). 15 g of N,N-dimethyl-4-bromo-2-methyl-3-nitroaniline is obtained as a brownish-orange oil.

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후처리

  1. temperatureheated to 90° C.-100° C
  2. extractionthe aqueous phase is extracted with 300 ml of ether
  3. washThe organic phase is washed with Na2CO3 (1M)
  4. filtrationfiltered
  5. customevaporated down
  6. customThe product is purified by chromatography (silica gel, eluant

출처 및 근거

ORD 기록
ord-41cae8c194804849a1a2181d90428e73
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06602897B2

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