Trifluoroacetic acid → HCID 66711490, 화합물

HRID 1262124노트

반응식

HRID 1262124 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[CH:19]=[CH:18][C:17]([NH:20][C:21]3[N:26]=[CH:25][C:24]4=[CH:27][CH:28]=[C:29]([C:30]5[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=5[O:36][CH3:37])[N:23]4[N:22]=3)=[C:16]([O:38][CH3:39])[CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:37][O:36][C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=1[C:29]1[N:23]2[C:24]([CH:25]=[N:26][C:21]([NH:20][C:17]3[CH:18]=[CH:19][C:14]([CH:11]4[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]4)=[CH:15][C:16]=3[O:38][CH3:39])=[N:22]2)=[CH:27][CH:28]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66711689HCID 66711689, 화합물

생성물 1

HCID 66711490HCID 66711490, 화합물수율 96%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-{3-Methoxy-4-[7-(2-methoxy-phenyl)-pyrrolo[2,1-f][1,2,4]triazin-2-ylamino]-phenyl}-piperidine-1-carboxylic acid tert-butyl ester (650.00 mg, 1.227 mmol) was treated with trifluoroacetic acid (0.473 mL, 6.136 mmol) in methylene chloride (3 mL) at room temperature until complete reaction of starting material was observed by hplc analysis of reaction mixture. The reaction was quenched with minimum amount of saturated aqueous sodium carbonate, and was extracted extensively in dichloromethane. The combined organic extracts were dried over MgSO4 and then filtered. Evaporation of solvent under reduced pressure afforded [7-(2-methoxy-phenyl)-pyrrolo[2,1-f][1,2,4]triazin-2-yl]-(2-methoxy-4-piperidin-4-yl-phenyl)-amine as a yellow foam (504 mg, 96%) which was used without further purification in the next step.

후처리

  1. customwas observed by hplc analysis of reaction mixture
  2. customThe reaction was quenched with minimum amount of saturated aqueous sodium carbonate
  3. extractionwas extracted extensively in dichloromethane
  4. dry with materialThe combined organic extracts were dried over MgSO4
  5. filtrationfiltered
  6. customEvaporation of solvent under reduced pressure

출처 및 근거

ORD 기록
ord-559ac83657a44784afcb8301aea163b3
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08471005B2

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