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Tetrahydrofuran → (S)-1-(1-(tert-butyldimethylsilyloxy)pent-4-en-2-yl)-3-(2-chloro-3-fluorobenzyl)-1-methylurea

HRID 340960
ノート
印刷プレビュー

反応式

HRID 340960 の反応式
[CH:1]1[C:6]([N+:7]([O-])=O)=[CH:5][CH:4]=[C:3]([Cl-]C([O-])=O)C=1.Cl.[Cl:15][C:16]1[C:23]([F:24])=[CH:22][CH:21]=[CH:20][C:17]=1[CH2:18][NH2:19].[CH3:25]CN(C(C)C)C(C)C.[Si:34]([O:41]C[C@@H](NC)CC=C)([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:36])[CH3:35].C1C[O:52][CH2:51]C1>>[Si:34]([O:41][CH2:1][C@@H:6]([N:7]([CH3:25])[C:51]([NH:19][CH2:18][C:17]1[CH:20]=[CH:21][CH:22]=[C:23]([F:24])[C:16]=1[Cl:15])=[O:52])[CH2:5][CH:4]=[CH2:3])([C:37]([CH3:38])([CH3:39])[CH3:40])([CH3:35])[CH3:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 8028Tetrahydrofuran3 回HCID 81531DiisopropylethylamineHCID 57947450(S)-1-(tert-butyldimethylsilyloxy)-N-methylpent-4-en-2-amineHCID 66622557(2-Chloro-3-fluorophenyl)methanamine hydrochloride

生成物 1

HCID 57947454(S)-1-(1-(tert-butyldimethylsilyloxy)pent-4-en-2-yl)-3-(2-chloro-3-fluorobenzyl)-1-methylurea収率 76%

実験手順

To a solution of 4-nitrophenylchloroformate (7.69 g, 38.3 mmol) in THF (20 mL) was added a solution of 2-chloro-3-fluorobenzylamine hydrochloride (6.09 g, 38.3 mmol) and DIEA (7.9 mL, 47.9 mmol) in THF (20 mL). The resulting solution was stirred at RT for 20 min. The reaction mixture was added into a solution of (S)-1-(tert-butyldimethylsilyloxy)-N-methylpent-4-en-2-amine (31.9 mmol) in THF (100 mL). The resulting solution was stirred at RT overnight. The solvent was removed and the resulting residue was re-dissolved in EtOAc (500 mL). The organic mixture was washed with NaOH (1 N, 100 mL×3), HCl (0.5 N, 100 mL), saturated NaHCO3, and brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified on silica gel column using a mixture of DCM and MeOH to give (S)-1-(1-(tert-butyldimethylsilyloxy)pent-4-en-2-yl)-3-(2-chloro-3-fluorobenzyl)-1-methylurea (10.08 g, 76%) as a white solid. LRMS (M+H+) m/z 415.2.

後処理

  1. stirringThe resulting solution was stirred at RT overnight
  2. customThe solvent was removed
  3. dissolutionthe resulting residue was re-dissolved in EtOAc (500 mL)
  4. washThe organic mixture was washed with NaOH (1 N, 100 mL×3), HCl (0.5 N, 100 mL), saturated NaHCO3, and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified on silica gel column
  9. additiona mixture of DCM and MeOH

出典と根拠

ORDレコード
ord-f08aa5aba64f455c932b06c7e3395d79
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895582B2

反応ノート

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