Hydrochloric Acid → HCID 21997570, 화합물

HRID 1977259노트

반응식

HRID 1977259 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=1.[CH3:19][O-:20].[Na+].Cl>CO>[CH3:19][O:20][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 21997456HCID 21997456, 화합물

생성물 1

HCID 21997570HCID 21997570, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of methyl 4-(6-bromo-n-hexyloxy)benzoate (186 g) in methanol (1 L) was treated with 28% sodium methoxide in methanol (340 ml) and the solution refluxed for 2 hours. After cooling, the stirred solution was adjusted to pH 2 with 1M-hydrochloric acid then extracted with ethyl acetate. The organic layer was washed with water, dried over magnesium sulfate, filtered and evaporated to give a crude oil. This oil was purified on a silica gel column (2 kg, 9:1 hexane-ethyl acetate elution) to give methyl 4-(6-methoxy-n-hexyloxy)benzoate (127 g) as an oil.

후처리

  1. temperaturethe solution refluxed for 2 hours
  2. temperatureAfter cooling
  3. extractionthen extracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customto give a crude oil
  9. customThis oil was purified on a silica gel column (2 kg, 9:1 hexane-ethyl acetate elution)

출처 및 근거

ORD 기록
ord-204068cd6dd44ce880ace9fed018fc57
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232290B1

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