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Methyl bromoacetate → Methyl 2-(5-((2,4,6-trimethoxystyrylsulfonyl)methyl)-2-methoxyphenylamino)acetate

HRID 424350
ノート
印刷プレビュー

反応式

HRID 424350 の反応式
Br[CH2:2][C:3]([O:5][CH3:6])=[O:4].C([O-])(=O)C.[Na+].[CH3:12][O:13][C:14]1[CH:34]=[C:33]([O:35][CH3:36])[CH:32]=[C:31]([O:37][CH3:38])[C:15]=1/[CH:16]=[CH:17]/[S:18]([CH2:21][C:22]1[CH:23]=[CH:24][C:25]([O:29][CH3:30])=[C:26]([NH2:28])[CH:27]=1)(=[O:20])=[O:19]>CO>[CH3:12][O:13][C:14]1[CH:34]=[C:33]([O:35][CH3:36])[CH:32]=[C:31]([O:37][CH3:38])[C:15]=1[CH:16]=[CH:17][S:18]([CH2:21][C:22]1[CH:23]=[CH:24][C:25]([O:29][CH3:30])=[C:26]([NH:28][CH2:2][C:3]([O:5][CH3:6])=[O:4])[CH:27]=1)(=[O:20])=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 60984Methyl bromoacetateHCID 517045Sodium AcetateHCID 11486204(E)-2-methoxy-5-(((2,4,6-trimethoxystyryl)sulfonyl)methyl)aniline

生成物 1

HCID 76144830Methyl 2-(5-((2,4,6-trimethoxystyrylsulfonyl)methyl)-2-methoxyphenylamino)acetate収率 85%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred solution of methyl bromoacetate (5 mmol) and sodium acetate (5 mmol) in methanol (20 mL) was added (E)-5-((2,4,6-trimethoxystyrylsulfonyl)methyl)-2-methoxybenzenamine (1 mmol). The resulting mixture was heated to reflux temperature. The heated mixture was stirred at reflux temperature for 12 to 15 h. The heated mixture was then cooled and poured onto water ice (about 100 g). A precipitate formed. The precipitate was separated by filtration to provide the product in 85% yield. m.p. 182-185° C.

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux temperature
  3. temperatureat reflux temperature for 12 to 15 h
  4. temperatureThe heated mixture was then cooled
  5. additionpoured onto water ice (about 100 g)
  6. customA precipitate formed
  7. customThe precipitate was separated by filtration
  8. customto provide the product in 85% yield

出典と根拠

ORDレコード
ord-d6f136bb62de4ca191bfcf41a5396f25
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08106033B2

反応ノート

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