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Oxalyl chloride → 4-[2-(Benzofurazan-5-yl)ethyl]-1-(indole-5-carbonyl)piperazine

HRID 1195677
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HRID 1195677 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([C:10]([OH:12])=O)=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.C(Cl)(=O)C(Cl)=O.[N:19]1[O:23][N:22]=[C:21]2[CH:24]=[C:25]([CH2:28][CH2:29][N:30]3[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]3)[CH:26]=[CH:27][C:20]=12.C(N(C(C)C)CC)(C)C>C1COCC1.CN(C=O)C.ClCCl>[N:19]1[O:23][N:22]=[C:21]2[CH:24]=[C:25]([CH2:28][CH2:29][N:30]3[CH2:31][CH2:32][N:33]([C:10]([C:6]4[CH:5]=[C:4]5[C:9](=[CH:8][CH:7]=4)[NH:1][CH:2]=[CH:3]5)=[O:12])[CH2:34][CH2:35]3)[CH:26]=[CH:27][C:20]=12
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참가 물질

8

반응물 4

HCID 65578Oxalyl chlorideHCID 742801H-Indole-5-Carboxylic AcidHCID 81531DiisopropylethylamineHCID 151663825-(2-Piperazin-1-ylethyl)-2,1,3-benzoxadiazole

생성물 1

HCID 151663954-[2-(Benzofurazan-5-yl)ethyl]-1-(indole-5-carbonyl)piperazine

시약·촉매·용매 3

HCID 6228
Dimethylformamide
촉매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매

실험 절차

Indole-5-carboxylic acid (57 mg, 0.35 mmol) was dissolved in THF (2 ml) and DMF (1 drop), then oxalyl chloride (37 μl, 54 mg, 0.42 mmol) was added. The mixture was stirred at room temperature for 3 hours, the solvent was evaporated under reduced pressure and the residue was dissolved in DMF (2 ml) and added to a stirred solution of 1-[2-(benzofurazan-5-yl)ethyl]piperazine (81 mg, 0.35 mmol) and diisopropylethylamine (91 μl, 68 mg, 0.52 mmol) in dichloromethane (1 ml). The mixture was stirred at room temperature for 24 hours, then the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with CH2Cl2 /CH3OH/NH3 ; 96:4:0.4 and crystallized from ethyl acetate/CHCl3 /hexane to give the piperazine as yellow microcrystals (16 mg, 12%), mp 180°-183° C.

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in DMF (2 ml)
  3. stirringThe mixture was stirred at room temperature for 24 hours
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by flash column chromatography on silica gel
  6. washeluting with CH2Cl2 /CH3OH/NH3
  7. custom96:4:0.4 and crystallized from ethyl acetate/CHCl3 /hexane

출처 및 근거

ORD 기록
ord-c929f49f7a3c4bd08781344c509356af
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05112824

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