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Water → HCID 45117061, 화합물

HRID 2111003
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HRID 2111003 반응식
[CH:1]1[C:6]([CH2:7][Cl:8])=[CH:5][CH:4]=[C:3](/[C:9](/Cl)=[N:10]\[OH:11])[CH:2]=1.CO[CH:15]=[CH:16][C:17]([O:19][CH3:20])=[O:18].C(N(CC)CC)C.O>ClCCl>[Cl:8][CH2:7][C:6]1[CH:5]=[CH:4][C:3]([C:9]2[C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][O:11][N:10]=2)=[CH:2][CH:1]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 2724617Methyl 3-methoxyprop-2-enoateHCID 91622765HCID 91622765, 화합물

생성물 1

HCID 45117061HCID 45117061, 화합물수율 51.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

N-Hydroxy-4-chloromethylbenzenecarboxyimidoyl chloride (15.27 g, 74.82 mmol) was dissolved in dichloromethane (300 ml), methyl 3-methoxyacrylate (10.43 g, 89.82 mmol) was added, and triethylamine (21 ml, 151 mmol) was slowly added dropwise. The mixture was stirred overnight at room temperature. Water was added, and the mixture was extracted with dichloromethane. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the obtained crude product was purified by silica gel chromatography (hexane:ethyl acetate=5:1) to give the title compound (9.67 g, 51%).

후처리

  1. extractionthe mixture was extracted with dichloromethane
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe obtained crude product
  6. customwas purified by silica gel chromatography (hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-a3a1861b58df4dc7b771d683206694cb
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07517996B2

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