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2-Aminoterephthalic acid → HCID 58574291, 화합물

HRID 1619420
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HRID 1619420 반응식
CO[C:3]1[CH2:4][CH2:5][CH:6]([CH3:10])[CH2:7][CH2:8][N:9]=1.[NH2:11][C:12]1[CH:20]=[C:19]([C:21]([OH:23])=[O:22])[CH:18]=[CH:17][C:13]=1[C:14](O)=[O:15]>CN(C=O)C.O>[CH3:10][CH:6]1[CH2:7][CH2:8][N:9]2[C:3](=[N:11][C:12]3[C:13]([C:14]2=[O:15])=[CH:17][CH:18]=[C:19]([C:21]([OH:23])=[O:22])[CH:20]=3)[CH2:4][CH2:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 27248222-Aminoterephthalic acidHCID 106068367-methoxy-4-methyl-3,4,5,6-tetrahydro-2H-azepine

생성물 1

HCID 58574291HCID 58574291, 화합물수율 2.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A solution of (E)-7-methoxy-4-methyl-3,4,5,6-tetrahydro-2H-azepine (1.1 g) and 2-aminoterephthalic acid (1.4 g, 7.7 mmol) in DMF (30 mL) was stirred at 100° C. for 4 h. After it was cooled to room temperature, the reaction was diluted with water (80 mL) and extracted with ethyl acetate (2×60 mL). The combined organic layers were washed with brine and dried over anhydrous sodium sulfate. After filtration and concentration, the crude product was purified by silica gel chromatography to give 47 mg of desired product.

후처리

  1. extractionextracted with ethyl acetate (2×60 mL)
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationAfter filtration and concentration
  5. customthe crude product was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-d3cc29cb9623404dbe51d24ff52bc8c3
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772301B2

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