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(Bis(2-methoxyethyl)amino)sulfur trifluoride → HCID 58387952, 화합물

HRID 2079954
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HRID 2079954 반응식
COCCN(S(F)(F)[F:11])CCOC.[CH3:14][O:15][C:16](=[O:27])[C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24]O)=[N:19][C:18]=1[NH2:26]>ClCCl>[CH3:14][O:15][C:16](=[O:27])[C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][F:11])=[N:19][C:18]=1[NH2:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2734690(Bis(2-methoxyethyl)amino)sulfur trifluorideHCID 58387955HCID 58387955, 화합물

생성물 1

HCID 58387952HCID 58387952, 화합물수율 7.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of (bis(2-methoxyethyl)amino)sulfur trifluoride (2.39 g, 10.8 mmol) in dichloromethane (30 mL) was cooled with a dry ice-methanol bath, and 2-amino-6-(2-hydroxyethyl)-nicotinic acid methyl ester (50 mg, 0.255 mmol) was added thereto dropwise. After dropwise addition the cold bath was immediately removed, and the solution was gradually allowed to room temperature. Water and ethyl acetate were added to the reaction solution, which was then partitioned. The organic layer was separated, the solvent was evaporated in vacuo, the residue was purified by silica gel column chromatography, and the title compound (4 mg, 0.020 mmol, 7.9%) was obtained as a white solid.

후처리

  1. additionAfter dropwise addition the cold bath
  2. customwas immediately removed
  3. customwas gradually allowed to room temperature
  4. additionWater and ethyl acetate were added to the reaction solution, which
  5. customwas then partitioned
  6. customThe organic layer was separated
  7. customthe solvent was evaporated in vacuo
  8. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-bb8ac51043154bfcbcaf2574f8c54f47
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932272B2

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