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Trifluoroacetic acid → HCID 23653974、化合物

HRID 1666641
ノート
印刷プレビュー

反応式

HRID 1666641 の反応式
NN1CCCC1.[C:7]1([CH2:13][C:14]([N:16]2[CH2:20][CH2:19][C@H:18]([NH:21][C:22]3[N:31]=[C:30]([N:32]4[CH2:37][CH2:36][N:35](C(OC(C)(C)C)=O)[CH2:34][CH2:33]4)[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[N:23]=3)[CH2:17]2)=[O:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.FC(F)(F)C(O)=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[C:7]1([CH2:13][C:14]([N:16]2[CH2:20][CH2:19][C@H:18]([NH:21][C:22]3[N:31]=[C:30]([N:32]4[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]4)[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[N:23]=3)[CH2:17]2)=[O:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 279461-PyrrolidinamineHCID 57970218HCID 57970218、化合物

生成物 1

HCID 23653974HCID 23653974、化合物収率 71.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a mixture of t-butyl 4-(2-((S)-pyrrolidin-3-ylamino)quinazolin-4-yl)piperazine-1-carboxylate (0.15 g), pyridine (60 mg), and chloroform was added phenylacetic acid chloride (87 mg), and the mixture was stirred at room temperature for 16 h. To the reaction mixture was added saturated aqueous sodium hydrogencarbonate, the mixture was extracted with chloroform, and the organic layer was dried with anhydrous magnesium sulfate. The desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, and then the residue was purified by silica gel column chromatography (NH silica gel, hexane/ethyl acetate=2:1−ethyl acetate) to obtain t-butyl 4-(2-((S)-1-(2-phenylethanoyl)pyrrolidin-3-ylamino)quinazolin-4-yl)piperazine-1-carboxylate (0.12 g). (2) To t-butyl 4-(2-((S)-1-(2-phenylethanoyl)pyrrolidin-3-ylamino)quinazolin-4-yl)piperazine-1-carboxylate (0.12 g) was added a mixed solution (7.5 mL) of chloroform and trifluoroacetic acid (10:1), and the mixture was stirred overnight at room temperature. To the reaction mixture was added 1 M aqueous sodium hydroxide, the mixture was extracted with chloroform, and the organic layer was dried with anhydrous magnesium sulfate. The desiccant was removed by filtration, then the solvent was evaporated, and the residue was purified by preparative TLC to obtain title compound (69 mg).

後処理

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialthe organic layer was dried with anhydrous magnesium sulfate
  3. customThe desiccant was removed by filtration
  4. customthe solvent was evaporated
  5. customthe residue was purified by preparative TLC

出典と根拠

ORDレコード
ord-87d1e0332f364547a2871ca914bed6c9
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044068B2

反応ノート

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