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

HRID 424350
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HRID 424350 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d6f136bb62de4ca191bfcf41a5396f25
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106033B2

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