Diisopropylethylamine → HCID 71060455、化合物

HRID 1036693ノート

反応式

HRID 1036693 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 71060455HCID 71060455、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-b5cac5635fbd44439f33eb10fa7d5d59
出典データセット
uspto-grants-2013_10
特許番号
US08546416B2

反応ノート

読み込み中…