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Hydrochloric Acid → HCID 58933648, 화합물

HRID 854295
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HRID 854295 반응식
[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][N:8]=[C:7](C=O)[CH:6]=1)[CH3:2].[CH:14]([O:21][CH2:22][CH3:23])([O:18][CH2:19][CH3:20])OCC.Cl.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:6]=[CH:7][N:8]=[C:9]([CH:14]([O:18][CH2:19][CH3:20])[O:21][CH2:22][CH3:23])[CH:10]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 31214Ethyl orthoformateHCID 19600808Ethyl 2-formylpyridine-4-carboxylate

생성물 1

HCID 58933648HCID 58933648, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
110 °C

실험 절차

To a solution of 2-formyl-isonicotinic acid ethyl ester (5.0 g, 0.027 mol) in ethanol (9 mL) was added triethyl orthoformate (6.2 mL, 0.037 mol) followed by a solution of 6N hydrochloric acid in ethanol (1.5 mL). The mixture was heated to 110° C. (reflux) for 1.5 h, cooled to rt and solid potassium carbonate (1.80 g) added. The mixture was stirred for 5 min, concentrated in vacuo, and redissolved in diethyl ether (100 mL). The reaction was filtered through silica and the resulting cake washed with diethyl ether (50 mL). The filtrated was concentrated in vacuo to give 2-diethoxymethyl-isonicotinic acid ethyl ester as an oil.

후처리

  1. temperature(reflux) for 1.5 h
  2. temperaturecooled to rt
  3. concentrationconcentrated in vacuo
  4. dissolutionredissolved in diethyl ether (100 mL)
  5. filtrationThe reaction was filtered through silica
  6. washthe resulting cake washed with diethyl ether (50 mL)
  7. concentrationThe filtrated was concentrated in vacuo

출처 및 근거

ORD 기록
ord-35c7d8501b4a40da83f010235aa1b3b6
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07259157B2

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