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N-methyl-2-pyrrolidone → 4-Chloro-1-(4-methylbenzene-1-sulfonyl)-3-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine

HRID 490275
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HRID 490275 반응식
[F-].[K+].CN1C(=O)CCC1.[Cl:10][C:11]1[CH:16]=[CH:15][N:14]=[C:13]2[N:17]([S:21]([C:24]3[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=3)(=[O:23])=[O:22])[CH:18]=[C:19](I)[C:12]=12.C[Si](C)(C)[C:33]([F:36])([F:35])[F:34]>[Cu]I.C(OC)(C)(C)C.CN(C=O)C>[Cl:10][C:11]1[CH:16]=[CH:15][N:14]=[C:13]2[N:17]([S:21]([C:24]3[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=3)(=[O:23])=[O:22])[CH:18]=[C:19]([C:33]([F:36])([F:35])[F:34])[C:12]=12
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참가 물질

8

반응물 4

HCID 13387N-methyl-2-pyrrolidoneHCID 522689Potassium Fluoride2회HCID 552549(Trifluoromethyl)trimethylsilaneHCID 53438252N-Tosyl-4-chloro-3-iodo-7-azaindole

생성물 1

HCID 116893174-Chloro-1-(4-methylbenzene-1-sulfonyl)-3-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine수율 67.3%

시약·촉매·용매 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
2회
HCID 6228Dimethylformamide용매
HCID 15413tert-Butyl methyl ether용매

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온도
220 °C

실험 절차

Under protective gas atmosphere (argon), 23.1 g (0.398 mol) of dry potassium fluoride and 75.7 g (0.398 mol) of copper(I) iodide were titrated together and heated to 220° C. under high vacuum with agitation for 10 minutes until a slightly greenish colouration appeared. A reaction flask was initially charged under protective gas atmosphere (argon) with the calcined mixture of potassium fluoride and copper(I) iodide together with 170 ml of absolute NMP and 170 ml of absolute DMF, and 86 g (0.199 mol) of 4-chloro-1-(toluene-4-sulphonyl)-3-iodo-1H-pyrrolo[2,3-b]pyridine were subsequently introduced in portions at 20° C. with stirring to form a light grey suspension. 62.1 g (0.437 mol) of trimethyltrifluoromethylsilane were added dropwise to the reaction mixture within 20 minutes and the mixture was left to stir at 20° C. for 18 h. On completion of conversion (GC monitoring of conversion), the reaction mixture was added to 2000 ml of methyl tert-butyl ether, the organic phase was decanted and the residue was dispersed once more with 1000 ml of methyl tert-butyl ether. The combined organic phases were washed three times with 2000 ml each time of water and subsequently dried over MgSO4. Filtration and removal of the volatile constituents in a water-jet vacuum resulted in 50.1 g (0.134 mol; 67%) of 4-chloro-1-(toluene-4-sulphonyl)-3-trifluoromethyl-1H-pyrrolo[2,3-b]pyridine as a beige solid.

후처리

  1. additionwere subsequently introduced in portions at 20° C.
  2. customto form a light grey suspension
  3. waitthe mixture was left
  4. stirringto stir at 20° C. for 18 h
  5. customthe organic phase was decanted
  6. additionthe residue was dispersed once more with 1000 ml of methyl tert-butyl ether
  7. washThe combined organic phases were washed three times with 2000 ml each time of water
  8. dry with materialsubsequently dried over MgSO4
  9. filtrationFiltration and removal of the volatile constituents in a water-jet vacuum

출처 및 근거

ORD 기록
ord-e97a8221d2e0457ba5ca59da07b5acf2
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07528146B2

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