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Diisopropylethylamine → HCID 178495706, 화합물

HRID 1413002
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HRID 1413002 반응식
[CH3:1][O:2][CH2:3][C@@H:4]1[CH2:8][N:7](C(OC(C)(C)C)=O)[C@H:6]([C:16]2[NH:17][C:18]([C:21]3[CH:26]=[C:25]4[CH2:27][O:28][C:29]5[CH:47]=[C:46]6[C:32]([CH:33]=[CH:34][C:35]7[N:39]=[C:38]([C@@H:40]8[CH2:44][CH2:43][C@H:42]([CH3:45])[NH:41]8)[NH:37][C:36]=76)=[CH:31][C:30]=5[C:24]4=[CH:23][CH:22]=3)=[CH:19][N:20]=2)[CH2:5]1.[CH3:48][O:49][C@H:50]([CH3:60])[C@H:51]([NH:55][C:56]([O:58][CH3:59])=[O:57])[C:52](O)=[O:53].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.C(=O)(O)[O-].[Na+]>CN(C=O)C>[CH3:59][O:58][C:56](=[O:57])[NH:55][C@@H:51]([C@H:50]([O:49][CH3:48])[CH3:60])[C:52]([N:41]1[C@@H:42]([CH3:45])[CH2:43][CH2:44][C@H:40]1[C:38]1[NH:37][C:36]2[C:46]3[C:32]([CH:33]=[CH:34][C:35]=2[N:39]=1)=[CH:31][C:30]1[C:24]2[C:25]([CH2:27][O:28][C:29]=1[CH:47]=3)=[CH:26][C:21]([C:18]1[NH:17][C:16]([C@@H:6]3[CH2:5][C@H:4]([CH2:3][O:2][CH3:1])[CH2:8][NH:7]3)=[N:20][CH:19]=1)=[CH:22][CH:23]=2)=[O:53]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 59540170(2S,3R)-3-methoxy-2-(methoxycarbonylamino)butanoic acidHCID 178495689HCID 178495689, 화합물

생성물 1

HCID 178495706
HCID 178495706, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of tert-butyl(2S,4S)-4-(methoxymethyl)-2-(5-{2-[(2S,5S)-5-methylpyrrolidin-2-yl]-1,11-dihydroisochromeno[4′,3′:6,7]naphtho[1,2-d]imidazol-9-yl}-1H-imidazol-2-yl)pyrrolidine-1-carboxylate (101 mg, 0.159 mmol), (2S,3R)-3-methoxy-2-(methoxycarbonylamino)butanoic acid (30 mg, 0.159 mmol), HATU (61 mg, 0.159 mmol) and 2 mL 10% DIPEA in DMF was stirred at room temperature for 1.5 hours. Saturated sodium bicarbonate was added and the product was extracted into dichloromethane, dried over sodium sulphate, filtered and concentrated under reduced pressure. This crude product was treated with 5 mL 1.25N HCl in ethanol at 50° C. for 4 h and then it was concentrated under reduced pressure. Saturated sodium bicarbonate was added and the product was extracted into dichloromethane, dried over sodium sulphate, filtered and concentrated under reduced pressure. (74.6 mg)

후처리

  1. extractionthe product was extracted into dichloromethane
  2. dry with materialdried over sodium sulphate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. additionThis crude product was treated with 5 mL 1.25N HCl in ethanol at 50° C. for 4 h
  6. concentrationit was concentrated under reduced pressure
  7. additionSaturated sodium bicarbonate was added
  8. extractionthe product was extracted into dichloromethane
  9. dry with materialdried over sodium sulphate
  10. filtrationfiltered
  11. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-257ae11e8e224a97af72e338b441c329
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921341B2

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