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Lithium Chloride → HCID 70664468、化合物

HRID 1186097
ノート
印刷プレビュー

反応式

HRID 1186097 の反応式
Cl[C:2]1[C:3]2[CH:31]=[C:30]([Cl:32])[CH:29]=[CH:28][C:4]=2[N:5]([CH2:19][C:20]2[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=2)[C:6](=[O:18])[CH:7]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=2[Cl:17])[N:8]=1.[Cl-].[Li+].O.[OH-].[Cs+].[CH3:38][O:39][C:40]1[CH:45]=[CH:44][C:43](B2OC(C)(C)C(C)(C)O2)=[CH:42][C:41]=1[CH3:55]>O1CCOCC1.O.C(OCC)(=O)C>[Cl:32][C:30]1[CH:29]=[CH:28][C:4]2[N:5]([CH2:19][C:20]3[CH:21]=[CH:22][C:23]([O:26][CH3:27])=[CH:24][CH:25]=3)[C:6](=[O:18])[CH:7]([CH2:9][C:10]3[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=3[Cl:17])[N:8]=[C:2]([C:43]3[CH:44]=[CH:45][C:40]([O:39][CH3:38])=[C:41]([CH3:55])[CH:42]=3)[C:3]=2[CH:31]=1
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 433294Lithium ChlorideHCID 21923912HCID 21923912、化合物HCID 23679066Caesium hydroxide--water (1/1/1)HCID 67060852HCID 67060852、化合物

生成物 1

HCID 70664468HCID 70664468、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 8857
Ethyl Acetate
溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
160 °C

実験手順

5,7-Dichloro-3-(2-chloro-4-fluorobenzyl)-1-(4-methoxybenzyl)-1H-benzo[e][1,4]diazepin-2(3H)-one (0.3 g, 0.61 mmol) was combined with lithium chloride (0.078 g, 1.83 mmol), cesium hydroxide hydrate (0.31 g, 1.83 mmol) and 2-(4-methoxy-3-methylphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.151 g, 0.61 mmol) in 1,4-dioxane (3 mL) and water (0.3 mL) and the mixture was purged with nitrogen. [Tetrakis(triphenylphosphine)]palladium(0) (0.07 g, 0.061 mmol) was added and the mixture was heated in a CEM Discover microwave reactor at 160° C. for 20 minutes. The mixture was allowed to cool and diluted with ethyl acetate then washed with water then brine. The organic layer was concentrated onto silica gel and chromatographed on a silica gel column eluting with 10-35% ethyl acetate in hexanes to give 7-chloro-3-(2-chloro-4-fluorobenzyl)-5-(4-methoxy-3-methylphenyl)-1-(4-methoxybenzyl)-1H-benzo[e][1,4]diazepin-2(3H)-one.

後処理

  1. customthe mixture was purged with nitrogen
  2. temperatureto cool
  3. washthen washed with water
  4. concentrationThe organic layer was concentrated onto silica gel
  5. customchromatographed on a silica gel column
  6. washeluting with 10-35% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-e8138bf435274d53a0214dae79825e33
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08673897B2

反応ノート

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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