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2-Bromobenzoic acid → 2-bromo-N,N-diethylbenzamide

HRID 1592707
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반응식

HRID 1592707 반응식
C1C=CC2N(O)N=NC=2C=1.[CH3:11][CH2:12][N:13](C(C)C)[CH:14](C)[CH3:15].[Br:20][C:21]1[CH:29]=[CH:28][CH:27]=[CH:26][C:22]=1[C:23]([OH:25])=O.C(NCC)C.CCN=C=NCCCN(C)C>C(Cl)Cl>[Br:20][C:21]1[CH:29]=[CH:28][CH:27]=[CH:26][C:22]=1[C:23]([N:13]([CH2:14][CH3:15])[CH2:12][CH3:11])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 69402-Bromobenzoic acidHCID 8021DiethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531Diisopropylethylamine

생성물 1

HCID 6690442-bromo-N,N-diethylbenzamide수율 129.8%

시약·촉매·용매 1

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
HCID 6344
Dichloromethane
용매

실험 절차

HOBT (2.72 g, 10.08 mmol), DIPEA (3.52 mL, 20.16 mmol), 2-bromo benzoic acid (4.08 g, 10.08 mmol), and diethyl amine (2.08 mL, 10.08 mmol) were dissolved in DCM (100 mL) and stirred at r.t. for about 30 minutes. EDCI (3.86 g, 10.08 mmol) was added, and the mixture was stirred at r.t. for about 16 hours. The reaction was concentrated to an oil, and the oil was purified via column chromatography to give 2-bromo-N,N-diethyl-benzamide (3.35 g, 68%) as a yellow oil.

후처리

  1. stirringthe mixture was stirred at r.t. for about 16 hours
  2. concentrationThe reaction was concentrated to an oil
  3. customthe oil was purified via column chromatography

출처 및 근거

ORD 기록
ord-a173b33f57344b8ba2c9460bd4ba0d1a
출처 데이터셋
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07291619B2

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