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Water → HCID 54066124, 화합물

HRID 341775
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HRID 341775 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH:11]=[C:10]([CH2:13][CH:14]([C:18]([OH:20])=[O:19])C(O)=O)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].O.[Cl-].[Na+].[CH3:24]N(C=O)C>>[C:1]([O:5][C:6]([N:8]1[CH2:12][CH:11]=[C:10]([CH2:13][CH2:14][C:18]([O:20][CH3:24])=[O:19])[CH2:9]1)=[O:7])([CH3:2])([CH3:3])[CH3:4]
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참가 물질

5

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HCID 962WaterHCID 5234Sodium ChlorideHCID 6228DimethylformamideHCID 69945705HCID 69945705, 화합물

생성물 1

HCID 54066124HCID 54066124, 화합물수율 92%

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온도
150 °C

실험 절차

To a solution of 4.52 g (14.4 mmol) 2-(1-tert.-butoxycarbonyl-2,5-dihydro-1H-pyrrol-3-yl-methyl)-malonic acid idimethylester n 140 ml DMF were added 1.94 g (108 mmol) water and 1.26 g( 21.6 mmol) sodium chloride. The mixture was degassed and heated to 150° C. for 30 h under an atmosphere of argon. After this period of time no starting material could be detected by TLC. The mixture was cooled to room temperature, diluted with 200 ml ether and washed three times with water, then with brine. The organic layer was dried over MgSO4 and evaporated. Purification by bulb-to-bulb distillation gave 3.38 g (92%) of 3-(2-methoxycarbonyl-ethyl)-2,5-dihydropyrrole-1-carboxylic acid tert. butylester as a colorless oil, b.p. 130° C. (0.2 mbar).

후처리

  1. customThe mixture was degassed
  2. waitAfter this period of time no starting material could be detected by TLC
  3. temperatureThe mixture was cooled to room temperature
  4. additiondiluted with 200 ml ether
  5. washwashed three times with water
  6. dry with materialThe organic layer was dried over MgSO4
  7. customevaporated
  8. customPurification
  9. distillationby bulb-to-bulb distillation

출처 및 근거

ORD 기록
ord-1a6bd0a0643742568286b72310b3c31a
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05856309

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