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Isobutyl chloroformate → HCID 86676204, 화합물

HRID 1052172
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HRID 1052172 반응식
[C:1]([O:5][C:6]([N:8]1[C@@H:16]2[C@@H:11]([CH2:12][CH2:13][CH2:14][CH2:15]2)[CH2:10][C@H:9]1[C:17](O)=[O:18])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(Cl)(=O)OCC(C)C.[NH2:28][C:29]1[CH:33]=[C:32]([Br:34])[S:31][C:30]=1[C:35]([NH2:37])=[O:36].C(=O)([O-])O.[Na+]>O1CCCC1.C(OCC)(=O)C.C(N(CC)CC)C>[Br:34][C:32]1[S:31][C:30]([C:35](=[O:36])[NH2:37])=[C:29]([NH:28][C:17]([C@@H:9]2[CH2:10][C@H:11]3[C@H:16]([CH2:15][CH2:14][CH2:13][CH2:12]3)[N:8]2[C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])=[O:18])[CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 62365Isobutyl chloroformateHCID 516892Sodium BicarbonateHCID 2755991(2S,3aS,7aS)-1-(tert-Butoxycarbonyl)octahydro-1H-indole-2-carboxylic acidHCID 219758623-Amino-5-bromothiophene-2-carboxamide

생성물 1

HCID 86676204HCID 86676204, 화합물수율 64.6%

시약·촉매·용매 3

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8471Triethylamine용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of (2S,3aS,7aS)-1-(tert-butoxycarbonyl) octahydro-1H-indole-2-carboxylic acid (638 mg) and triethylamine (0.392 mL) in tetrahydrofuran (5 mL) was added 2-methylpropyl chlorocarbonate (0.324 mL) at 0° C., and the mixture was stirred at room temperature for 30 min. Thereafter, to the reaction system was added a solution of 3-amino-5-bromothiophene-2-carboxamide (250 mg) produced in Example 1, step D, in tetrahydrofuran (5 mL), and the mixture was stirred at 60° C. for 26 hr. Ethyl acetate (20 mL) and aqueous sodium hydrogen carbonate (10 mL) were added to the reaction mixture, and the separated aqueous layer was extracted with ethyl acetate (5 mL). The combined organic layers were washed with brine (5 mL) and dried over anhydrous sodium sulfate. Insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane), and the object fraction was concentrated under reduced pressure to give the title compound (345 mg) as a pale-yellow amorphous solid.

후처리

  1. extractionthe separated aqueous layer was extracted with ethyl acetate (5 mL)
  2. washThe combined organic layers were washed with brine (5 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationInsoluble material was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
  7. concentrationthe object fraction was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7af430d7ea924ed0a7f3f0d3f8c12423
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388195B2

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