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Proton sponge → HCID 60083663, 화합물

HRID 1883149
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HRID 1883149 반응식
[C:1]([C@@H:3]([NH:6][C:7]([C@@H:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C@@H:10]1[NH:15][C:16]([C:18]1[N:19]([CH3:27])[C:20]2[C:25]([CH:26]=1)=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])=[O:8])[CH2:4][OH:5])#[N:2].F[B-](F)(F)F.[CH3:33][O+](C)C.CN(C1C2C(N(C)C)=CC=CC=2C=CC=1)C>ClCCl>[C:1]([C@@H:3]([NH:6][C:7]([C@@H:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C@@H:10]1[NH:15][C:16]([C:18]1[N:19]([CH3:27])[C:20]2[C:25]([CH:26]=1)=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])=[O:8])[CH2:4][O:5][CH3:33])#[N:2]
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참가 물질

5

반응물 3

HCID 88675Proton spongeHCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 60091030HCID 60091030, 화합물

생성물 1

HCID 60083663HCID 60083663, 화합물수율 38.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

N-[(1S,2R)-2-({[(1R)-1-Cyano-2-hydroxyethyl]amino}carbonyl)cyclohexyl]-1-methyl-1H-indole-2-carboxamide from Example 4 (0.20 g, 0.54 mmol) was dissolved in dichloromethane (8 mL), cooled to 0° C. under nitrogen in the dark, and stirred for 15 minutes. Trimethyloxonium tetrafluoroborate (0.10 g, 0.68 mmol) was added (Sowinski, J. A.; Toogood, P. L. J. Org. Chem. 1996, 61, 7671). After 20 minutes, proton sponge (0.14 g, 0.65 mmol) was added, and the reaction was allowed to warm to room temperature and was stirred for 21 hours. The reaction mixture was filtered through a pad of celite and the pad washed with dichloromethane. The filtrate was washed with 1M hydrochloric acid, brine, dried on magnesium sulfate, and concentrated. Purification by column chromatography (5:95 methanol:dichlormethane) gave 1-methyl-1H-indole-2-carboxylic acid {(1S,2R)-2-[((R)-cyano-methoxymethyl-methyl)-carbamoyl]-cyclohexyl}-amide (0.08 g, 38%). MS: 383 (M+H).

후처리

  1. waitAfter 20 minutes
  2. temperatureto warm to room temperature
  3. stirringwas stirred for 21 hours
  4. filtrationThe reaction mixture was filtered through a pad of celite
  5. washthe pad washed with dichloromethane
  6. washThe filtrate was washed with 1M hydrochloric acid, brine
  7. customdried on magnesium sulfate
  8. concentrationconcentrated
  9. customPurification by column chromatography (5:95 methanol:dichlormethane)

출처 및 근거

ORD 기록
ord-7b68b05b4de94ff6a7e4acc044e09be2
출처 데이터셋
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06759428B2

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