Hydrochloric Acid → [4-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]bromoacetic acid

HRID 963789노트

반응식

HRID 963789 반응식
[CH:1]([Br:4])(Br)Br.[Br-].[Li+].[OH-:7].[K+].[C:9]([C:11]1[CH:18]=[CH:17][C:14](C=O)=[C:13]([O:19][CH2:20][O:21][CH2:22][CH2:23][O:24][CH3:25])[C:12]=1[O:26][CH2:27][O:28][CH2:29][CH2:30][O:31][CH3:32])#[N:10].Cl.[O:34]1[CH2:39]COCC1>C(OCC)(=O)C.O>[C:9]([C:11]1[CH:18]=[CH:17][C:14]([CH:1]([Br:4])[C:39]([OH:34])=[O:7])=[C:13]([O:19][CH2:20][O:21][CH2:22][CH2:23][O:24][CH3:25])[C:12]=1[O:26][CH2:27][O:28][CH2:29][CH2:30][O:31][CH3:32])#[N:10]

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 5558BromoformHCID 14797Potassium HydroxideHCID 312751,4-DioxaneHCID 82050Lithium BromideHCID 183590784-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-benzaldehyde

생성물 1

HCID 18359186[4-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]bromoacetic acid

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

440 microliters of bromoform were added at -5° C. to a mixture of 4.26 mg of lithium bromide, 598 mg of potassium hydroxide and 5 ml of water and then, a solution of 825 mg of a 4-cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-benzaldehyde (preparation given hereafter) in 5 ml of dioxane was added dropwise. The mixture was stirred for 72 hours at 0° C. to -5° C. and was poured into a stirred mixture at 0° C. to -5° C. of 15 ml of ethyl acetate and 11 ml of hydrochloric acid. Extraction was carried out with ethyl acetate and the extracts were washed, dried and evaporated to dryness under reduced pressure. The oil obtained was used as is for the following step.

후처리

  1. extractionExtraction
  2. washthe extracts were washed
  3. customdried
  4. customevaporated to dryness under reduced pressure
  5. customThe oil obtained

출처 및 근거

ORD 기록
ord-5edfa31d22b64c1f840dff7b614031a6
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763617

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