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Methanol → 6-methoxy-7-(morpholinomethyl)benzofuran-3(2H)-one

HRID 1749793
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HRID 1749793 반응식
[OH:1][C:2]1[CH:11]=[CH:10][C:5]2[C:6](=[O:9])[CH2:7][O:8][C:4]=2[C:3]=1[CH2:12][N:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1.CO.[C:21]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O.C1(C)C=CC=CC=1>C1COCC1>[CH3:21][O:1][C:2]1[CH:11]=[CH:10][C:5]2[C:6](=[O:9])[CH2:7][O:8][C:4]=2[C:3]=1[CH2:12][N:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 887MethanolHCID 1140TolueneHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 712789376-hydroxy-7-(morpholinomethyl)benzofuran-3(2H)-one

생성물 1

HCID 712789876-methoxy-7-(morpholinomethyl)benzofuran-3(2H)-one수율 82.3%

시약·촉매·용매

1
HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 6-hydroxy-7-(morpholinomethyl)benzofuran-3(2H)-one (0.586 g, 2.35 mmol), methanol (0.0904 g, 2.82 mmol) and triphenylphosphine (0.923 g, 3.52 mmol) in THF (12 mL) was added with a solution of a 40% solution of diethyl azodicarboxylate in toluene (1.84 g, 4.23 mmol) in THF (6 mL), and the mixture was stirred overnight at room temperature. The reaction mixture was concentrated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol) to obtain 6-methoxy-7-(morpholinomethyl)benzofuran-3(2H)-one (0.509 g, 82%).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-2385507b304746d2a4ab31db500482de
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09156827B2

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