Disilathiane, 1,1,1,3,3,3-hexamethyl- → 3-[7-(4-Fluoro-phenyl)-4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-thiobenzamide

HRID 1062246

反応式

HRID 1062246 の反応式
N[C@H](C(O)=O)C([SH:6])(C)C.C[Si](C)(C)S[Si](C)(C)C.C[O-].[Na+].[F:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]2[CH:48]=[CH:47][C:32]3[N:33]=[C:34]([C:39]4[CH:40]=[C:41]([CH:44]=[CH:45][CH:46]=4)[C:42]#[N:43])[CH2:35][C:36](=[O:38])[NH:37][C:31]=3[CH:30]=2)=[CH:25][CH:24]=1>CN1CCN(C)C1=O.O>[F:22][C:23]1[CH:24]=[CH:25][C:26]([C:29]2[CH:48]=[CH:47][C:32]3[N:33]=[C:34]([C:39]4[CH:40]=[C:41]([CH:44]=[CH:45][CH:46]=4)[C:42]([NH2:43])=[S:6])[CH2:35][C:36](=[O:38])[NH:37][C:31]=3[CH:30]=2)=[CH:27][CH:28]=1

参加物

7

反応物 4

HCID 76920Disilathiane, 1,1,1,3,3,3-hexamethyl-HCID 92863L-PenicillamineHCID 97987263-[7-(4-Fluoro-phenyl)-4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-benzonitrileHCID 10942334Sodium Methoxide

生成物 1

HCID 222246273-[7-(4-Fluoro-phenyl)-4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-thiobenzamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 66611,3-Dimethyl-2-imidazolidinone溶媒2 回

実験手順

Preparation of 4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-thiobenzamides (according to Pen-Yuan Lin et al. Synthesis 1992, 1219]: To a solution of hexamethyldisilthiane (1.45 g, 8.0 mmol) in 1,3-dimethyl-2-imidazolidinone (8 mL) was added at 23° C. sodium methoxide (0.31 g, 6.8 mmol). The mixture was stirred for 5 min. and the blue solution formed was then added to a solution of 3-[7-(4-fluoro-phenyl)-4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-benzonitrile (Example 57) (1.42 g, 4 mmol) in 1,3-dimethyl-2-imidazolidinone (12 mL). The mixture was stirred for 3 h at 23° C. and then poured into water (100 mL). Stirring was continued for 0.5 h and the precipitate was isolated by filtration and triturated with ethyl acetate (50 mL) to give the title compound as light yellow solid (1.38 g).

後処理

  1. customthe blue solution formed
  2. stirringThe mixture was stirred for 3 h at 23° C.
  3. stirringStirring
  4. waitwas continued for 0.5 h
  5. customthe precipitate was isolated by filtration
  6. customtriturated with ethyl acetate (50 mL)

出典と根拠

ORDレコード
ord-309d7a701d63487faa01b1bb3ae5a48a
出典データセット
uspto-grants-2005_11
特許番号
US06960578B2

関連ノート

読み込み中…