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Diisopropylethylamine → HCID 69289368、化合物

HRID 2375792
ノート
印刷プレビュー

反応式

HRID 2375792 の反応式
[CH3:1][O:2][C:3]([CH2:5][CH2:6][C:7]1[C:8]([CH3:16])=[C:9]([C:13]([OH:15])=O)[NH:10][C:11]=1[CH3:12])=[O:4].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.Cl.Cl.[CH:52]([N:55]1[CH2:60][CH2:59][CH:58]([NH2:61])[CH2:57][CH2:56]1)([CH3:54])[CH3:53]>CN(C=O)C>[CH3:1][O:2][C:3](=[O:4])[CH2:5][CH2:6][C:7]1[C:8]([CH3:16])=[C:9]([C:13](=[O:15])[NH:61][CH:58]2[CH2:59][CH2:60][N:55]([CH:52]([CH3:54])[CH3:53])[CH2:56][CH2:57]2)[NH:10][C:11]=1[CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 81531Diisopropylethylamine2 回HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 108468134-(2-METHOXYCARBONYL-ETHYL)-3,5-DIMETHYL-1H-PYRROLE-2-CARBOXYLIC ACIDHCID 177503401-(Propan-2-yl)piperidin-4-amine dihydrochloride

生成物 1

HCID 69289368HCID 69289368、化合物
収率 40.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

263 mg of (1.17 mmol) 4-(2-methoxycarbonyl-ethyl)-3,5-dimethyl-1H-pyrrole-2-carboxylic acid were dissolved in DMF (10 mL). 488.4 mg (1.28 mmol) of HATU and DIEA (224 μl) were added and the resulting mixture was stirred for 45 minutes at RT. A solution of 276.3 mg (1.28 mmol) of 1-isopropyl-piperidine-4-ylamine-dihydrochloride and 448 μl of DIEA was added. The reaction mixture was stirred over night after which it was concentrated. The residue was diluted with DCM and washed with a saturated NaHCO3 solution and brine. The organic layer was dried over MgSO4 and concentrated. Preparative HPLC(CH3CN/H2O gradient+0.05% formic acid) gave pure 3-[5-(1-isopropyl-piperidin-4-ylcarbamoyl)-2,4-dimethyl-1H-pyrrol-3-yl]-propionic acid methyl ester (166 mg) as a colorless amorphous material. MS (ESI+): m/e=351 [M+H]+.

後処理

  1. stirringThe reaction mixture was stirred over night after which it
  2. concentrationwas concentrated
  3. additionThe residue was diluted with DCM
  4. washwashed with a saturated NaHCO3 solution and brine
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-6d6470a8dc5f4e32b5d88017b3cb7564
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07465806B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート