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Methanol → 2,4-Dichloro-6-methoxymethylbenzylamine

HRID 1481345
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HRID 1481345 반응식
[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[C:6]([CH2:11][O:12][CH3:13])[C:3]=1[C:4]#[N:5].CO.[OH-].[Na+]>C1COCC1>[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[C:6]([CH2:11][O:12][CH3:13])[C:3]=1[CH2:4][NH2:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 210220682,4-Dichloro-6-(methoxymethyl)benzonitrile

생성물 1

HCID 897047972,4-Dichloro-6-methoxymethylbenzylamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
60 °C

실험 절차

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

A solution of BH3 (3.5 mL, 1M in THF) was added to a solution of 2,4-dichloro-6-(methoxymethyl)benzonitrile (0.88 mmol) in 3 mL THF. The reaction mixture was heated to 60° C. for 2 h. At 0° C., 3.5 mL MeOH was dropwise added and the mixture was stirred until gas evolution was finished. An aq. solution of 10% NaOH was added still under cooling. The solvent was removed under vacuo, the residue was diluted with water and extracted 3 times with EtOAc. The combined organic layers were dried over MgSO4 and concentrated in vacuo to give the desired product as orange oil.

후처리

  1. temperatureunder cooling
  2. customThe solvent was removed under vacuo
  3. additionthe residue was diluted with water
  4. extractionextracted 3 times with EtOAc
  5. dry with materialThe combined organic layers were dried over MgSO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-427439c804e14e3f9aeb2294674b3934
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409917B2

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