Diisopropylethylamine → HCID 71060455, 화합물

HRID 1036693노트

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HRID 1036693 반응식
[C:1]([O:5][C:6]([N:8]([CH3:22])[C:9]([CH3:21])([CH3:20])[C:10](ON1C(=O)CCC1=O)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:23][C@H:24]([CH2:46][O:47][CH2:48][C:49]1[CH:54]=[CH:53][C:52]([CH3:55])=[CH:51][CH:50]=1)[C:25]([N:27]1[CH2:45][CH2:44][CH2:43][C:29]2([C:33](=[O:34])[N:32]([CH3:35])[CH2:31][CH:30]2[C:36]2[CH:41]=[CH:40][C:39]([F:42])=[CH:38][CH:37]=2)[CH2:28]1)=[O:26].CCN(C(C)C)C(C)C>C1COCC1.O>[F:42][C:39]1[CH:38]=[CH:37][C:36]([CH:30]2[C:29]3([CH2:43][CH2:44][CH2:45][N:27]([C:25](=[O:26])[C@H:24]([NH:23][C:10](=[O:11])[C:9]([N:8]([CH3:22])[C:6](=[O:7])[O:5][C:1]([CH3:3])([CH3:2])[CH3:4])([CH3:21])[CH3:20])[CH2:46][O:47][CH2:48][C:49]4[CH:54]=[CH:53][C:52]([CH3:55])=[CH:51][CH:50]=4)[CH2:28]3)[C:33](=[O:34])[N:32]([CH3:35])[CH2:31]2)=[CH:41][CH:40]=1

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 71060531HCID 71060531, 화합물HCID 866740982,5-Dioxopyrrolidin-1-yl 2-(tert-butoxycarbonyl(methyl)amino)-2-methylpropanoate

생성물 1

HCID 71060455HCID 71060455, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To 2,5-dioxopyrrolidin-1-yl 2-(tert-butoxycarbonyl(methyl)amino)-2-methylpropanoate (80 mg, 0.254 mmol) and 7-((R)-2-amino-3-(4-methylbenzyloxy)propanoyl)-4-(4-fluorophenyl)-2-methyl-2,7-diazaspiro[4.5]decan-1-one (115 mg, 0.254 mmol) in THF (3 ml) was added DIPEA (0.044 ml, 0.254 mmol) and the mixture stirred at RT overnight. The mixture was diluted with water (10 ml) and extracted with EtOAc (50 ml). The extracts were dried (MgSO4) and concentrated. The residue was applied to a 12 g silica cartridge which was eluted with ethyl acetate. The appropriate fractions were combined and concentrated to give tert-butyl 1-((2R)-1-(4-(4-fluorophenyl)-2-methyl-1-oxo-2,7-diazaspiro[4.5]decan-7-yl)-3-(4-methylbenzyloxy)-1-oxopropan-2-ylamino)-2-methyl-1-oxopropan-2-yl(methyl)carbamate as a foam.

후처리

  1. extractionextracted with EtOAc (50 ml)
  2. dry with materialThe extracts were dried (MgSO4)
  3. concentrationconcentrated
  4. washwas eluted with ethyl acetate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b5cac5635fbd44439f33eb10fa7d5d59
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546416B2

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