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Methanol → 2-Morpholin-4-ylmethyl-6-nitro-benzoic acid

HRID 874864
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인쇄 미리보기

반응식

HRID 874864 반응식
C[O:2][C:3](=[O:20])[C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:13][N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1.[OH-].[Na+].CO.C1COCC1>O>[N:14]1([CH2:13][C:5]2[CH:6]=[CH:7][CH:8]=[C:9]([N+:10]([O-:12])=[O:11])[C:4]=2[C:3]([OH:20])=[O:2])[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 598410552-Morpholin-4-ylmethyl-6-nitro-benzoic acid methyl ester

생성물 1

HCID 598410692-Morpholin-4-ylmethyl-6-nitro-benzoic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

A solution of compound 5 (0.85 g) and NaOH (0.304 g) in a mixture of water (9 mL), methanol (5 mL), and THF (45 mL) was stirred at reflux for 24 h and concentrated to dryness. The residue was dissolved in water, and the solution was cooled to 0° C. and adjusted to pH 7 with 10% potassium hydrogen sulfate. The mixture was concentrated to dryness, the residue was treated with methanol, and filtered to remove solids. The filtrate was concentrated to yield compound 6 as a yellow solid.

후처리

  1. temperatureat reflux for 24 h
  2. concentrationconcentrated to dryness
  3. dissolutionThe residue was dissolved in water
  4. concentrationThe mixture was concentrated to dryness
  5. additionthe residue was treated with methanol
  6. filtrationfiltered
  7. customto remove solids
  8. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-d3e40048ce104f5591afb3dc08250bbc
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08980901B2

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