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Hydrochloric Acid → 4-Bromo-2-[(3-ethoxy-3-oxopropanoyl)(propan-2-yl)amino]benzoic acid

HRID 1754557
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반응식

HRID 1754557 반응식
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[CH:3]=1.C(N(CC)CC)C.[Cl-].[C:23]([O:29][CH2:30][CH3:31])(=[O:28])[CH2:24][C:25]([O-])=[O:26].Cl>C(Cl)Cl>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([N:11]([C:25](=[O:26])[CH2:24][C:23]([O:29][CH2:30][CH3:31])=[O:28])[CH:12]([CH3:14])[CH3:13])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 22464965Ethyl malonate chlorideHCID 248246474-Bromo-2-(isopropylamino)benzoic acid

생성물 1

HCID 866798024-Bromo-2-[(3-ethoxy-3-oxopropanoyl)(propan-2-yl)amino]benzoic acid수율 72%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To a solution of 4-bromo-2-(propan-2-ylamino)benzoic acid (6.8 g, 26.64 mmol) in 260 mL of DCM is added triethylamine (4 mL, 31.6 mmol), followed by dropwise addition of ethyl malonate chloride (4.0 mL, 31. mmol). The mixture is stirred for 2 hours at room temperature, and then poured into molar hydrochloric acid solution and extracted with EtOAc. The organic phase is washed with water and with saturated aqueous NaCl solution, dried over Na2SO4 and concentrated to dryness. 7.15 g of a pale yellow solid are obtained (yield: 72%).

후처리

  1. extractionextracted with EtOAc
  2. washThe organic phase is washed with water and with saturated aqueous NaCl solution
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-b31ad14ad9db474baa0600e1a45f6bca
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09169246B2

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