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1-[(2-methoxyethoxy)methoxy]-4-nitroBenzene → 4-[(2-Methoxyethoxy)methoxy]aniline

HRID 2274245
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HRID 2274245 반응식
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=1>CO.[Pd]>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][C:8]1[CH:9]=[CH:10][C:11]([NH2:14])=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 196090861-[(2-methoxyethoxy)methoxy]-4-nitroBenzene

생성물 1

HCID 131356894-[(2-Methoxyethoxy)methoxy]aniline수율 98%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a suspension of Pd/C (0.5 g) in methanol (25 mL), 1-[(2-methoxyethoxy)methoxy]-4-nitrobenzene (2.35 g) was added to a 50 mL 3-neck RBF at room temperature under nitrogen atmosphere. Hydrogen gas was bubbled through the reaction mixture for 1-2 hr at room temperature and the reaction was monitored on TLC using chloroform:methanol (9.8:0.2) as mobile phase. After completion, the reaction mixture was filtered using Celite and washed with methanol. The combined filtrate was concentrated under reduced pressure at 40° C. to give 2.0 g of 4-[(2-methoxyethoxy)methoxy]aniline as a dark brown liquid.

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후처리

  1. additionwas added to a 50 mL 3-neck RBF at room temperature under nitrogen atmosphere
  2. customHydrogen gas was bubbled through the reaction mixture for 1-2 hr at room temperature
  3. filtrationAfter completion, the reaction mixture was filtered
  4. washwashed with methanol
  5. concentrationThe combined filtrate was concentrated under reduced pressure at 40° C.

출처 및 근거

ORD 기록
ord-13d1e85f0fac419cadcb41a79039d911
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09126950B2

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