Diisopropylethylamine → HCID 71075489、化合物

HRID 2170708ノート

反応式

HRID 2170708 の反応式
[CH3:1][O:2][C:3](=[O:28])[C@@H:4]([O:6][C:7]1[CH:8]=[C:9]([CH:25]=[CH:26][CH:27]=1)[CH2:10][N:11]1[C:19]2[C:14](=[CH:15][C:16]([C:20]([OH:22])=O)=[CH:17][CH:18]=2)[C:13]([CH3:23])=[C:12]1[CH3:24])[CH3:5].[CH:29]([O:32][C:33]1[CH:34]=[C:35]([C@@H:39]([NH2:41])[CH3:40])[CH:36]=[CH:37][CH:38]=1)([CH3:31])[CH3:30].CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>C(Cl)Cl>[CH:29]([O:32][C:33]1[CH:34]=[C:35]([C@@H:39]([NH:41][C:20]([C:16]2[CH:15]=[C:14]3[C:19](=[CH:18][CH:17]=2)[N:11]([CH2:10][C:9]2[CH:8]=[C:7]([CH:27]=[CH:26][CH:25]=2)[O:6][C@@H:4]([CH3:5])[C:3]([O:2][CH3:1])=[O:28])[C:12]([CH3:24])=[C:13]3[CH3:23])=[O:22])[CH3:40])[CH:36]=[CH:37][CH:38]=1)([CH3:31])[CH3:30]

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 28307561HCID 28307561、化合物HCID 71075220HCID 71075220、化合物

生成物 1

HCID 71075489HCID 71075489、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of (S)-1-(3-((1-methoxy-1-oxopropan-2-yl)oxy)benzyl)-2,3-dimethyl-1H-indole-5-carboxylic acid (50 mg, 0.13 mmol, 1 equiv) in DCM (2 mL) was added (S)-1-(3-isopropoxyphenyl)ethanamine (34 mg, 0.16 mmol, 1.2 equiv), DIEA (70 μL, 0.39 mmol, 3 equiv) and HATU (50 mg, 0.13 mmol, 1 equiv). The reaction mixture was stirred 2 h at room temperature. The solvent was removed in vacuo. The residue was dissolved in AcOEt and washed with a 0.5N HCl aqueous solution, a saturated NaHCO3 solution and brine, dried over MgSO4. The filtrate was concentrated to obtain the crude product which was purified by flash chromatography (AcOEt/Hexane 0->50%) to obtain the title compound.

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in AcOEt
  3. washwashed with a 0.5N HCl aqueous solution
  4. dry with materiala saturated NaHCO3 solution and brine, dried over MgSO4
  5. concentrationThe filtrate was concentrated
  6. customto obtain the crude product which
  7. customwas purified by flash chromatography (AcOEt/Hexane 0->50%)

出典と根拠

ORDレコード
ord-e0e8a60f5e7e493dbf90d494acc5dc41
出典データセット
uspto-grants-2015_06
特許番号
US09051265B2

反応ノート

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