Trifluoroacetic acid → HCID 66711490、化合物

HRID 1262124ノート

反応式

HRID 1262124 の反応式
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

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 66711689HCID 66711689、化合物

生成物 1

HCID 66711490HCID 66711490、化合物収率 96%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-559ac83657a44784afcb8301aea163b3
出典データセット
uspto-grants-2013_06
特許番号
US08471005B2

反応ノート

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