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Trifluoroacetic acid → HCID 18926538、化合物

HRID 1600187
ノート
印刷プレビュー

反応式

HRID 1600187 の反応式
FC(F)(F)C(O)=O.[CH3:8][O:9][C:10]([CH2:12][CH2:13][N:14]1[C:22]2[C:17](=[CH:18][C:19]([CH2:23][CH2:24][C:25]([O:27]C(C)(C)C)=[O:26])=[CH:20][CH:21]=2)[C:16]([CH2:32][C:33]2[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=2)=[CH:15]1)=[O:11]>ClCCl>[C:25]([CH2:24][CH2:23][C:19]1[CH:18]=[C:17]2[C:22](=[CH:21][CH:20]=1)[N:14]([CH2:13][CH2:12][C:10]([O:9][CH3:8])=[O:11])[CH:15]=[C:16]2[CH2:32][C:33]1[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=1)([OH:27])=[O:26]
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 18926564HCID 18926564、化合物

生成物 1

HCID 18926538HCID 18926538、化合物収率 86.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (15 ml) was added to a stirred solution of t-butyl 1-(2-methoxycarbonylethyl)-3-(3-pyridylmethyl)-1H-indole-5-propanoate (7.60 g) in dry dichloromethane (100 ml) at room temperature, and stirringwas continued for 18 hours. The solution was evaporated and the residue wasazeotroped with toluene and then dissolved in ethyl acetate. Saturated sodium bicarbonate solution was added slowly with shaking until the pH of the aqueous layer was 4-5. The organic layer was then separated, washed with water and dried (MgSO4). The solvent was evaporated and the residue was triturated with ether to give the title compound (5.70 g), m.p. 108°-110° C. Found: C,68.80; H,6.16; N,7.57%. C21 H22N2O4 requires: C,68.83; H,6.05; N,7.65%.

後処理

  1. customThe solution was evaporated
  2. dissolutiondissolved in ethyl acetate
  3. additionSaturated sodium bicarbonate solution was added slowly
  4. customThe organic layer was then separated
  5. washwashed with water
  6. dry with materialdried (MgSO4)
  7. customThe solvent was evaporated
  8. customthe residue was triturated with ether

出典と根拠

ORDレコード
ord-b8e6ed3465804b15a6080513d1e86e59
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05744488

反応ノート

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