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Acetonitrile → (R)-N-(bis(3-(trifluoromethoxy)phenyl)-methylene)-2-methylpropane-2-sulfinamide

HRID 1874161
ノート
印刷プレビュー

反応式

HRID 1874161 の反応式
[C:1](#[N:3])[CH3:2].[Li+].CC([N-]C(C)C)C.[F:12][C:13]([F:41])([F:40])[O:14][C:15]1[CH:16]=[C:17]([C:21]([C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([O:35][C:36]([F:39])([F:38])[F:37])[CH:30]=2)=[N:22][S@@:23]([C:25]([CH3:28])([CH3:27])[CH3:26])=[O:24])[CH:18]=[CH:19][CH:20]=1.[NH4+].[Cl-]>CCOCC.CCOC(C)=O>[F:39][C:36]([F:37])([F:38])[O:35][C:31]1[CH:30]=[C:29]([C:21]([C:17]2[CH:18]=[CH:19][CH:20]=[C:15]([O:14][C:13]([F:41])([F:40])[F:12])[CH:16]=2)=[N:22][S@@:23]([C:25]([CH3:28])([CH3:27])[CH3:26])=[O:24])[CH:34]=[CH:33][CH:32]=1.[C:1]([CH2:2][C:21]([NH:22][S@@:23]([C:25]([CH3:28])([CH3:27])[CH3:26])=[O:24])([C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([O:35][C:36]([F:37])([F:38])[F:39])[CH:30]=1)[C:17]1[CH:18]=[CH:19][CH:20]=[C:15]([O:14][C:13]([F:40])([F:41])[F:12])[CH:16]=1)#[N:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 6342AcetonitrileHCID 25517Ammonium ChlorideHCID 2724682Lithium diisopropylamideHCID 59458920(R)-N-(bis(3-(trifluoromethoxy)phenyl)-methylene)-2-methylpropane-2-sulfinamide

生成物 2

HCID 59458920(R)-N-(bis(3-(trifluoromethoxy)phenyl)-methylene)-2-methylpropane-2-sulfinamide
HCID 59459074
(R)-N-(2-cyano-1,1-bis(3-(trifluoromethoxy)phenyl)ethyl)-2-methylpropane-2-sulfinamide

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
-78 °C

実験手順

(R)—N-(bis(3-(trifluoromethoxy)phenyl)methylene)-2-methylpropane-2-sulfinamide was prepared as described for Procedure 11. Under an argon atmosphere, acetonitrile (0.46 mL, 8.84 mmol, 2.0 eq) was stirred in anhydrous Et2O (40 mL) in an oven-dried round bottomed flask at −78° C. LDA (2.0 M, 4.42 mL, 8.84 mmol, 2.0 eq) was added dropwise. The resulting mixture was stirred at −78° C. for 30 min. (R)—N-(bis(3-(trifluoromethoxy)phenyl)methylene)-2-methylpropane-2-sulfinamide (2.0 g, 4.42 mmol) in Et2O (10 mL) was added dropwise to the above stirred solution. The reaction mixture was stirred at −78° C. for 4 h. Sat'd NH4Cl was added, followed by the addition of EtOAc. The organic layer was washed with H2O and brine, dried over Na2SO4, filtered, and concentrated to dryness. The residue was purified by flash chromatography (silica gel, EtOAc/Hexanes=0 to 100%) to give (R)—N-(2-cyano-1,1-bis(3-(trifluoromethoxy)phenyl)ethyl)-2-methylpropane-2-sulfinamide as light tan oil (1.15 g, yield: 52.7% with 0.85 g recovery of the starting material). LC-MS (ESI) 495.26 (M+H), retention time=3.84 min (10-90% MeOH in H2O with 0.1% TFA in a 4-min run); 1H NMR (400 MHz, CDCl3) δ ppm 7.40-7.35 (m, 2H), 7.29 (d, J=8 Hz, 1H), 7.21-7.16 (m, 4H), 7.08 (m, 1H), 4.53 (s, 1H), 3.75 (d, J=16 Hz, 1H) 3.56 (d, J=16 Hz, 1H), 1.21 (s, 9H).

後処理

  1. additionwas added dropwise to the above stirred solution
  2. washThe organic layer was washed with H2O and brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated to dryness
  6. customThe residue was purified by flash chromatography (silica gel, EtOAc/Hexanes=0 to 100%)

出典と根拠

ORDレコード
ord-01d9e71c0d034d088bdd8eecac7bf0ef
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08304403B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート