Acetone → HCID 21221128、化合物

HRID 1377174

反応式

HRID 1377174 の反応式
[CH3:1][O:2][C:3]1[C:10]([O:11][CH3:12])=[C:9]([O:13][CH3:14])[CH:8]=[CH:7][C:4]=1[CH2:5]Cl.CC(C)=O.[I-:19].[Na+]>CCOCC>[CH3:1][O:2][C:3]1[C:10]([O:11][CH3:12])=[C:9]([O:13][CH3:14])[CH:8]=[CH:7][C:4]=1[CH2:5][I:19]

参加物

5

反応物 3

HCID 180AcetoneHCID 5238Sodium IodideHCID 97491Toluene, alpha-chloro-2,3,4-trimethoxy-

生成物 1

HCID 21221128HCID 21221128、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

46.64 g (215.2 mmol) of 2,3,4-trimethoxybenzyl chloride in 466 ml of abs. acetone are treated with 156.7 g (4.86 equivalents) of sodium iodide, and this mixture is stirred at RT for 2.75 h while excluding light. The reaction mixture is treated with approximately 3 l of (cold) ether, and the organic phase is washed once with 10 sodium thiophosphate solution and twice with saline (both kinds of solutions being cold). The combined aqueous phases are reextracted with ether. The combined organic phases are dried over Na2SO4 and evaporated on a RE at approximately 30° C. The residue, which is the desired title compound, is dried again under HV and subjected to further processing as a crude product. 1H-NMR (200 MHz, CDCl3): 7.03 and 6.59 (each d; each 1H); 4.47 (s, 2H); 4.05, 3.85 and 3.84 (each s, each 3H).

後処理

  1. washthe organic phase is washed once with 10 sodium thiophosphate solution and twice with saline (both kinds of solutions
  2. dry with materialThe combined organic phases are dried over Na2SO4
  3. customevaporated on a RE at approximately 30° C
  4. customis dried again under HV

出典と根拠

ORDレコード
ord-650d00b895b846988f0a51b96bfbbc18
出典データセット
uspto-grants-1997_09
特許番号
US05663200

関連ノート

読み込み中…