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Oxazole → Dimethyl 5-(oxazol-2-yl)isophthalate

HRID 2071132
ノート
印刷プレビュー

反応式

HRID 2071132 の反応式
[O:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[Li]CCCC.I[C:12]1[CH:13]=[C:14]([C:22]([O:24][CH3:25])=[O:23])[CH:15]=[C:16]([CH:21]=1)[C:17]([O:19][CH3:20])=[O:18]>C1COCC1.CCOC(C)=O.O.[Cl-].[Cl-].[Zn+2].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[O:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:12]1[CH:21]=[C:16]([C:17]([O:19][CH3:20])=[O:18])[CH:15]=[C:14]([CH:13]=1)[C:22]([O:24][CH3:25])=[O:23]
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 3

HCID 9255OxazoleHCID 2758568Dimethyl 5-iodoisophthalateHCID 178418339Butyllithium

生成物 1

HCID 11379968Dimethyl 5-(oxazol-2-yl)isophthalate収率 54%

試薬・触媒・溶媒 5

HCID 3007855Zincchloride触媒HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

To a stirred solution of oxazole ((0.28 mL, 4.2 mmol) in THF (10 mL) at −78° C. was added nBuLi (2.8 mL 1.6 N solution in hexane, 4.4 mmol). ZnCl2 (20 mL 0.5M soln, 10 mmol) was added after 30 min and the reaction mixture was warmed up to 0° C. for 1 h. To the resulting mixture was added dimethyl 5-iodoisophthalate (1.28 g, 4.0 mmol) and Pd(PPh3)4 and was heated at reflux for 5 h. The reaction mixture was cooled to room temperature and diluted with EtOAc and H2O. The layers were separated and the organic layer was washed with, brine, dried with Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography (20% EtOAc in hexanes) to provide dimethyl 5-(oxazol-2-yl)isophthalate (568 mg, 54%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 5 h
  3. temperatureThe reaction mixture was cooled to room temperature
  4. customThe layers were separated
  5. washthe organic layer was washed with, brine
  6. dry with materialdried with Na2SO4
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by column chromatography (20% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-c0a42131807d4676b485b615686e5698
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08299267B2

反応ノート

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