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

HRID 1058258
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HRID 1058258 반응식
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
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참가 물질

9

반응물 5

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

생성물 1

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

시약·촉매·용매 3

HCID 1068Dimethyl Sulfide용매HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

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온도
-50 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-9b343139991e417b97e35ba684dcb4dc
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06515011B2

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