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m-Chloroperbenzoic acid → HCID 90308809, 화합물

HRID 2283664
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HRID 2283664 반응식
C1C=C(Cl)C=C(C(OO)=O)C=1.[S:12]1[CH:16]=[CH:15][C:14]2[C:17]([NH:21][C:22]3[N:23]=[C:24](SC)[N:25]=[N:26][C:27]=3[C:28]([O:30][CH2:31][CH3:32])=[O:29])=[CH:18][CH:19]=[CH:20][C:13]1=2.[C:35]([O:39][C:40](=[O:49])[NH:41][C@H:42]1[CH2:47][CH2:46][CH2:45][CH2:44][C@H:43]1[NH2:48])([CH3:38])([CH3:37])[CH3:36].C(N(C(C)C)CC)(C)C>C(Cl)(Cl)Cl.C(OCC)(=O)C>[S:12]1[CH:16]=[CH:15][C:14]2[C:17]([NH:21][C:22]3[N:23]=[C:24]([NH:48][C@@H:43]4[CH2:44][CH2:45][CH2:46][CH2:47][C@@H:42]4[NH:41][C:40]([O:39][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:49])[N:25]=[N:26][C:27]=3[C:28]([O:30][CH2:31][CH3:32])=[O:29])=[CH:18][CH:19]=[CH:20][C:13]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 70297m-Chloroperbenzoic acidHCID 81531DiisopropylethylamineHCID 1514389(1S,2R)-Cyclohexane-1,2-diamine, N1-BOC protectedHCID 90308829HCID 90308829, 화합물

생성물 1

HCID 90308809HCID 90308809, 화합물

시약·촉매·용매 2

HCID 6212Chloroform
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

A solution of m-CPBA (65 mg) in chloroform (1.5 ml) was added to a solution of ethyl 5-(benzo[b]thiophen-4-ylamino)-3-(methylthio)-1,2,4-triazine-6-carboxylate obtained in the above-described Step 1 (33 mg) in chloroform (1.5 ml), the reaction solution was stirred at room temperature for 10 minutes. Thereafter, tert-butyl((1S,2R)-2-aminocyclohexyl)carbamate (60 mg) and diisopropylethylamine (0.10 ml) were added, and then the reaction solution was stirred at room temperature for 3 hours. The reaction solution was diluted with ethyl acetate and then washed successively with an aqueous sodium bicarbonate solution and a saturated saline solution. After drying over anhydrous sodium sulfate, the solvent was evaporated under vacuum, and then the resultant residue was purified by column chromatography on silica gel (developing solvent:hexane/ethyl acetate) to obtain ethyl 5-(benzo[b]thiophen-4-ylamino)-3-((1R,2S)-2-(tert-butoxycarbonylamino)cyclohexylamino)-1,2,4-triazine-6-carboxylate.

후처리

  1. stirringthe reaction solution was stirred at room temperature for 3 hours
  2. washwashed successively with an aqueous sodium bicarbonate solution
  3. dry with materialAfter drying over anhydrous sodium sulfate
  4. customthe solvent was evaporated under vacuum
  5. customthe resultant residue was purified by column chromatography on silica gel (developing solvent:hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-382a6ce8351a46e9ae0e951a7ee9560e
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09145414B2

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