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

HRID 1977285

反応式

HRID 1977285 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 20395Fenbutrazate溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-3922bb71b3ae40dc9c6c6221f25629ac
出典データセット
uspto-grants-2001_05
特許番号
US06232290B1

関連ノート

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