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Potassium Carbonate → Tert-butyl-[3-(5-fluoro-2-methoxy-4-nitro-phenoxy)-propoxy]-dimethyl-silane

HRID 1667769
ノート
印刷プレビュー

反応式

HRID 1667769 の反応式
[F:1][C:2]1[C:3]([N+:11]([O-:13])=[O:12])=[CH:4][C:5]([O:9][CH3:10])=[C:6]([OH:8])[CH:7]=1.Br[CH2:15][CH2:16][CH2:17][O:18][Si:19]([C:22]([CH3:25])([CH3:24])[CH3:23])([CH3:21])[CH3:20].C(=O)([O-])[O-].[K+].[K+].[Cl-].[NH4+]>CN(C)C=O>[C:22]([Si:19]([O:18][CH2:17][CH2:16][CH2:15][O:8][C:6]1[CH:7]=[C:2]([F:1])[C:3]([N+:11]([O-:13])=[O:12])=[CH:4][C:5]=1[O:9][CH3:10])([CH3:20])[CH3:21])([CH3:24])([CH3:25])[CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 607486(3-Bromopropoxy)(tert-butyl)dimethylsilaneHCID 67426546HCID 67426546、化合物

生成物 1

HCID 67428158Tert-butyl-[3-(5-fluoro-2-methoxy-4-nitro-phenoxy)-propoxy]-dimethyl-silane収率 69.8%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A mixture of 0.350 g (1.87 mmole) of 5-fluoro-2-methoxy-4-nitro-phenol, 0.568 g (2.25 mmole) of (3-bromo-propoxy)-tert-butyl-dimethyl-silane, 1.29 g (9.35 mmole) of potassium carbonate and 5 mL of dimethylformamide was heated at 60 degrees for 3 hours. The mixture was cooled, poured into 50 mL of dilute ammonium chloride solution and extracted three times with 25 mL of ethyl acetate. The combined organic extracts were washed three times with 25 mL of water, once with 25 mL of brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography, eluting with dichloromethane-hexanes (60:40) to give 0.469 g of tert-butyl-[3-(5-fluoro-2-methoxy-4-nitro-phenoxy)-propoxy]-dimethyl-silane (IV.42) as a white solid.

後処理

  1. temperaturewas heated at 60 degrees for 3 hours
  2. temperatureThe mixture was cooled
  3. extractionextracted three times with 25 mL of ethyl acetate
  4. washThe combined organic extracts were washed three times with 25 mL of water
  5. dry with materialonce with 25 mL of brine, dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel chromatography
  9. washeluting with dichloromethane-hexanes (60:40)

出典と根拠

ORDレコード
ord-087fb06fdbae407490f4b9ec4d10671f
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044213B2

反応ノート

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