Hydrochloric Acid → 1-Bromo-4-(7-methoxyheptylthio)benzene

HRID 1977285노트

반응식

HRID 1977285 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]Br)=[CH:4][CH:3]=1.[CH3:17][O-:18].[Na+].Cl>CO.CCC(C(OCCN1C(C)C(C2C=CC=CC=2)OCC1)=O)C1C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][O:18][CH3:17])=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 219974831-Bromo-4-(7-bromoheptylthio)benzene

생성물 1

HCID 219975631-Bromo-4-(7-methoxyheptylthio)benzene

시약·촉매·용매 2

HCID 887Methanol용매HCID 20395Fenbutrazate용매

실험 절차

To a solution of 1-bromo-4-(7-bromoheptylthio)benzene (5 g) in methanol (25 ml) was added 28% sodium mehtylate in nethanol (7.9 g) and the mixture was stirred under refluxing for 2 hours. The residue was adjusted to pH 2 with dilute HCl aq. and extracted with ethyl acetate. The organic layer was seperated, wahsed with brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (50:1) to give 1-bromo-4-(7-methoxyheptylthio)benzene (3.59 g).

후처리

  1. temperatureunder refluxing for 2 hours
  2. extractionextracted with ethyl acetate
  3. customThe organic layer was seperated
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (50:1)

출처 및 근거

ORD 기록
ord-3922bb71b3ae40dc9c6c6221f25629ac
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232290B1

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