Dimethylformamide → 4-Octyloxy-benzo[1,3]dioxole

HRID 18448

反応式

HRID 18448 の反応式
[CH2:1]1[O:5][C:4]2[CH:6]=[C:7](O)[CH:8]=[CH:9][C:3]=2[O:2]1.[H-].[Na+].Br[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21].CN(C=[O:26])C>>[CH2:14]([O:26][C:6]1[C:4]2[O:5][CH2:1][O:2][C:3]=2[CH:9]=[CH:8][CH:7]=1)[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 81401-BromooctaneHCID 24758Sodium hydrideHCID 68289Sesamol

生成物 1

HCID 685862504-Octyloxy-benzo[1,3]dioxole

実験手順

A solution of sesamol (6.9 g; 50 mmol) in DMF (100 mL) under N2 was cooled to 0° C. and sodium hydride (60% w/w dispersion; 2.3 g; 60 mmol) carefully added. The slurry was allowed to warm to room temperature over 1 hour after which time 1-bromooctane (13 mL; 75 mmol) was added. The mixture was stirred for 5 days, poured onto H2O and extracted with diethylether (2×). The combined organic fractions were dried (MgSO4), filtered and evaporated in vacuo to yield 12.8 g (quantitative yield) of a white solid. Mp. 120° C.

後処理

  1. additionwas added
  2. additionpoured onto H2O
  3. extractionextracted with diethylether (2×)
  4. dry with materialThe combined organic fractions were dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-b2c6d3a3cb494844a131ef9e2c03dda4
出典データセット
uspto-grants-2010_06
特許番号
US07741352B2

関連ノート

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