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Trifluoroacetic acid → HCID 18926538, 화합물

HRID 1600187
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HRID 1600187 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 18926564HCID 18926564, 화합물

생성물 1

HCID 18926538HCID 18926538, 화합물수율 86.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-b8e6ed3465804b15a6080513d1e86e59
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05744488

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