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Ammonium Hydroxide → 4-(4-Chloro-2-{[(triisopropylsilyl)oxy]methyl}phenyl)azetidin-2-one

HRID 1058258
ノート
印刷プレビュー

反応式

HRID 1058258 の反応式
C([Li])CCC.[Cl:6][C:7]1[CH:8]=[CH:9][C:10](I)=[C:11]([CH:24]=1)[CH2:12][O:13][Si:14]([CH:21]([CH3:23])[CH3:22])([CH:18]([CH3:20])[CH3:19])[CH:15]([CH3:17])[CH3:16].C(O[CH:30]1[NH:33][C:32](=[O:34])[CH2:31]1)(=O)C.[Cl-].[NH4+].[OH-].[NH4+]>CCOCC.CSC.C1COCC1>[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([CH:30]2[NH:33][C:32](=[O:34])[CH2:31]2)=[C:11]([CH2:12][O:13][Si:14]([CH:21]([CH3:23])[CH3:22])([CH:18]([CH3:20])[CH3:19])[CH:15]([CH3:17])[CH3:16])[CH:24]=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

9

反応物 5

HCID 14923Ammonium HydroxideHCID 25517Ammonium ChlorideHCID 1199814-Acetoxy-2-azetidinoneHCID 18672361[(5-Chloro-2-iodobenzyl)oxy](triisopropyl)silaneHCID 178418339Butyllithium

生成物 1

HCID 186723524-(4-Chloro-2-{[(triisopropylsilyl)oxy]methyl}phenyl)azetidin-2-one収率 86%

試薬・触媒・溶媒 3

HCID 1068Dimethyl Sulfide溶媒HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-50 °C

実験手順

n-Butyl-lithium (2.5 M solution in hexanes, 3.6 mL) was added to stirred solution of [(5-chloro-2-iodobenzyl)oxy](triisopropyl)silane (3.82 g, 9.0 mmol) in ether (18 mL) at −78° C. under nitrogen. After 10 min a solution of copper(I) bromide-dimethylsulfide complex (0.925 g, 4.5 mmol) in dimethylsulfide (36 mL) was added and the solution was warmed to −50° C. A solution of 4-acetoxy-2-azetidinone (0.291 g, 2.25 mmol) in THF (2 mL) was added and the solution was warmed to −30° C. After a further 1 h the reaction was poured into 10% ammonium chloride solution basicified with ammonium hydroxide and extracted into ether. The organic layer was dried (Na2SO4) and evaporated in vacuo to an oil which was purified by flash column chromatography on silica (eluting with 5% methylene chloride/0-50% ethyl acetate/hexanes gradient) to give 4-(4-chloro-2-{[(triisopropylsilyl)oxy]methyl}phenyl)azetidin-2-one (0.712 g) as a heavy oil: 1H NMR (CDCl3, 400 MHz) δ 1.08 (d, J=6.4 Hz, 18H), 1.16 (septet, J=6.4 Hz, 3H), 2.78 (dd, J=2.6, 14.8 Hz, 1H), 3.45 (dq, J=14.8, 2.6 Hz, 1H), 4.72 (d, J=13.1 Hz, 1H), 4.78 (d, J=13.1 Hz, 1H), 4.94 (q, J=2.6 Hz, 1H), 6.06 (br s, 1H), 7.30 (dd, J=2.1, 8.4 Hz, 1H), 7.43 (m, 2H).

後処理

  1. temperaturethe solution was warmed to −30° C
  2. extractionextracted into ether
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. customevaporated in vacuo to an oil which
  5. customwas purified by flash column chromatography on silica (eluting with 5% methylene chloride/0-50% ethyl acetate/hexanes gradient)

出典と根拠

ORDレコード
ord-9b343139991e417b97e35ba684dcb4dc
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06515011B2

反応ノート

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