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Triethylamine → HCID 21884460, 화합물

HRID 722492
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HRID 722492 반응식
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][C:4]=1[N+:12]([O-:14])=[O:13].[Br:15][C:16]1[CH:21]=[CH:20][C:19]([OH:22])=[C:18]([NH2:23])[CH:17]=1.C(N(CC)CC)C>C1COCC1>[OH:22][C:19]1[CH:20]=[CH:21][C:16]([Br:15])=[CH:17][C:18]=1[NH:23][C:7](=[O:8])[C:6]1[CH:10]=[CH:11][C:3]([O:2][CH3:1])=[C:4]([N+:12]([O-:14])=[O:13])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 3518402-Amino-4-BromophenolHCID 123754634-Methoxy-3-nitrobenzoyl chloride

생성물 1

HCID 21884460HCID 21884460, 화합물수율 43.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 4-methoxy-3-nitro-benzoyl chloride (7.12 g, 33.0 mmol) in THF (50 ml) was added dropwise with stirring to a solution of 4-bromo-2-aminophenol (6.20 g, 33.0 mmol) in THF (50 ml) containing triethylamine (6.82 ml, 66.0 mmol). After addition was complete the reaction was stirred at room temperature overnight. The reaction mixture was concentrated to approximately half the original volume and the precipitate collected by filtration. The solid was washed with methanol and ether and dried under vacuum to give the subtitle compound as a brown solid (5.24 g, 42%). 1H NMR (DMSO) δ 8.58(d, 1H), 8.36(dd, 1H), 7.55(d, 1H), 6.96(m, 2H), 6.68(dd, 1H), 4.05(s, 3H).

후처리

  1. additionAfter addition
  2. concentrationThe reaction mixture was concentrated to approximately half the original volume
  3. filtrationthe precipitate collected by filtration
  4. washThe solid was washed with methanol and ether
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-56e172ca16ef445890f1efcdc0a25a01
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07138425B2

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