Cyclopropylamine → 9H-fluoren-9-ylmethyl 2-[(cyclopropylamino)carbonyl]morpholine-4-carboxylate

HRID 1435500ノート

反応式

HRID 1435500 の反応式
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH:25]1([NH2:28])[CH2:27][CH2:26]1.[CH:29]1[C:41]2[CH:40]([CH2:42][O:43][C:44]([N:46]3[CH2:51][CH2:50][O:49][CH:48]([C:52](O)=[O:53])[CH2:47]3)=[O:45])[C:39]3[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=3)[C:33]=2[CH:32]=[CH:31][CH:30]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[CH:25]1([NH:28][C:52]([CH:48]2[O:49][CH2:50][CH2:51][N:46]([C:44]([O:43][CH2:42][CH:40]3[C:39]4[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=4[C:33]4[C:41]3=[CH:29][CH:30]=[CH:31][CH:32]=4)=[O:45])[CH2:47]2)=[O:53])[CH2:27][CH2:26]1

参加物

6

反応物 4

HCID 69828CyclopropylamineHCID 81531DiisopropylethylamineHCID 27561284-{[(9H-fluoren-9-yl)methoxy]carbonyl}morpholine-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

生成物 1

HCID 579373209H-fluoren-9-ylmethyl 2-[(cyclopropylamino)carbonyl]morpholine-4-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

HATU (1.17 g, 3.0 mmol) and cyclopropylamine (0.17 g, 3.0 mmol) were added to a solution of 4-[(9H-fluoren-9-ylmethoxy)carbonyl]morpholine-2-carboxylic acid (1.0 g, 2.9 mmol) and DIPEA (0.56 mL, 3.2 mmol) in DMF (50 mL). The reaction mixture was stirred for 2 hrs. at ambient temperature and the solvent was concentrated. The product was recovered in EtOAc and washed with water, saturated NaHCO3 solution, water and brine. The organic layer was dried over anhydrous MgSO4 and the solvent was concentrated to provide the title compound that was used for the next step without further purification. MS (ESI) (M+H)+=393.0.

後処理

  1. concentrationat ambient temperature and the solvent was concentrated
  2. customThe product was recovered in EtOAc
  3. washwashed with water, saturated NaHCO3 solution, water and brine
  4. dry with materialThe organic layer was dried over anhydrous MgSO4
  5. concentrationthe solvent was concentrated

出典と根拠

ORDレコード
ord-188770e5ffba4498836c524f6fb63420
出典データセット
uspto-grants-2009_11
特許番号
US07615642B2

反応ノート

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