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Trifluoroacetic acid → HCID 15985573、化合物

HRID 2193148
ノート
印刷プレビュー

反応式

HRID 2193148 の反応式
C(OC(=O)[N:7]([CH:19]1[CH2:24][CH2:23][N:22]([CH2:25][CH2:26][N:27]2[C:36]3[C:31](=[C:32](Br)[CH:33]=[C:34]([O:37][CH3:38])[CH:35]=3)[CH:30]=[CH:29][C:28]2=[O:40])[CH2:21][CH2:20]1)[CH2:8][C:9]1[CH:18]=[CH:17][C:12]2[O:13][CH2:14][CH2:15][O:16][C:11]=2[CH:10]=1)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[O:13]1[C:12]2[CH:17]=[CH:18][C:9]([CH2:8][NH:7][CH:19]3[CH2:24][CH2:23][N:22]([CH2:25][CH2:26][N:27]4[C:36]5[C:31](=[CH:32][CH:33]=[C:34]([O:37][CH3:38])[CH:35]=5)[CH:30]=[CH:29][C:28]4=[O:40])[CH2:21][CH2:20]3)=[CH:10][C:11]=2[O:16][CH2:15][CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 59397948tert-butyl (1-(2-(5-bromo-7-methoxy-2-oxoquinolin-1(2H)-yl)ethyl)piperidin-4-yl)(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)carbamate

生成物 1

HCID 15985573HCID 15985573、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 2 mL of a dichloromethane solution containing 20 mg of tert-butyl(1-(2-(5-bromo-7-methoxy-2-oxoquinolin-1(2H)-yl)ethyl)piperidin-4- yl)(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)carbamate, 1 mL of trifluoroacetic acid was added and stirred at room temperature for 2 hours. The solvent was removed under reduced pressure, chloroform and water were added, and adjusted to pH 13 with 20% aqueous sodium hydroxide solution. The organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and extracts were combined, washed with aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to give 16 mg of 5-bromo-1-(2-(4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl-7-methoxyquinolin-2(1H)-one as a light brown oil.

後処理

  1. additionwas added
  2. customThe solvent was removed under reduced pressure, chloroform and water
  3. additionwere added
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted with chloroform
  6. washwashed with aqueous saturated sodium chloride solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-5a0a4795337140b680196ad8a255275d
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08329694B2

反応ノート

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