Acetone → HCID 21221128, 화합물

HRID 1377174

반응식

HRID 1377174 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 21221128HCID 21221128, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-650d00b895b846988f0a51b96bfbbc18
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05663200

연결된 노트

불러오는 중…