Methylamine → 4-chloro-2-(hydroxymethyl)-N-methylbenzamide

HRID 2252817노트

반응식

HRID 2252817 반응식
[CH3:1][NH2:2].[Cl:3][C:4]1[CH:13]=[CH:12][C:7]2[C:8](=[O:11])[O:9][CH2:10][C:6]=2[CH:5]=1>CO>[Cl:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]([NH:2][CH3:1])=[O:11])=[C:6]([CH2:10][OH:9])[CH:5]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 2417375-Chloro-1,3-dihydro-2-benzofuran-1-one

생성물 1

HCID 691802354-chloro-2-(hydroxymethyl)-N-methylbenzamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methylamine gas was condensed into a sealed tube at −78° C., and a solution of 5-chloro-2-benzofuran-1(3H)-one (6.68 g, 39.8 mmol) in methanol (30 mL) was added. The solution was slowly warmed to room temperature overnight; The reaction was concentrated in vacuo, and the residue was partitioned between water and and chloroform. After three extractions with chloroform, the combined organics were dried over sodium sulfate, filtered, and concentrated in vacuo to afford 4-chloro-2-(hydroxymethyl)-N-methylbenzamide.

후처리

  1. customcondensed into a sealed tube at −78° C.
  2. concentrationThe reaction was concentrated in vacuo
  3. customthe residue was partitioned between water and and chloroform
  4. extractionAfter three extractions with chloroform
  5. dry with materialthe combined organics were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-55e528e2c8444b6191108304948f3a54
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07323460B2

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