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Pyridine → HCID 22346411, 화합물

HRID 897331
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HRID 897331 반응식
C([O:9][C:10]1[C:19]2[N:18]=[CH:17][CH:16]=[CH:15][C:14]=2[C:13](=[O:20])[NH:12][C:11]=1[C:21]([O:23][CH3:24])=[O:22])(=O)C1C=CC=CC=1.N1C=CC=CC=1.[O:31](S(C(F)(F)F)(=O)=O)[S:32]([C:35]([F:38])([F:37])[F:36])(=O)=[O:33]>ClCCl>[OH:9][C:10]1[C:11]([C:21]([O:23][CH3:24])=[O:22])=[N:12][C:13]([O:20][S:32]([C:35]([F:38])([F:37])[F:36])(=[O:33])=[O:31])=[C:14]2[C:19]=1[N:18]=[CH:17][CH:16]=[CH:15]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 22346242HCID 22346242, 화합물

생성물 1

HCID 22346411HCID 22346411, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a stirring suspension of the compound of Step 2 (25 g, 77 mmol) in dry dichoromethane (150 ml) under argon was added pyridine (31 ml, 385 mmol). The suspension was then cooled to 0° C. and Tf2O (32.6 g, 19.4 ml, 116 mmol) was added dropwise which caused the formation of a red color. The ice bath was then removed and after 1 hour the red solution was poured into a saturated aqueous solution of NaHCO3 (200 ml). The organic phase was separated and the aqueous phase was extracted three times with chloroform. The combined organics were dried over sodium sulfate, filtered and concentrated to give a green solid.

후처리

  1. customThe ice bath was then removed and after 1 hour the red solution
  2. additionwas poured into a saturated aqueous solution of NaHCO3 (200 ml)
  3. customThe organic phase was separated
  4. extractionthe aqueous phase was extracted three times with chloroform
  5. dry with materialThe combined organics were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give a green solid

출처 및 근거

ORD 기록
ord-497d3110222e43a7aceb44e404f68e8a
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06921759B2

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