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Diisopropylethylamine → HCID 86677177, 화합물

HRID 929352
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HRID 929352 반응식
CC[N:3]([CH:7](C)C)C(C)C.[Cl:10][C:11]1[CH:12]=[N:13][C:14]2[C:19]([N:20]=1)=[CH:18][C:17]([C:21](Cl)=[O:22])=[CH:16][CH:15]=2.ClC1C=NC2C(=CC=C([C:35](Cl)=[O:36])C=2)N=1>C(Cl)Cl>[Cl:10][C:11]1[CH:12]=[N:13][C:14]2[C:19]([N:20]=1)=[CH:18][C:17]([C:21]([N:3]([O:36][CH3:35])[CH3:7])=[O:22])=[CH:16][CH:15]=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 20228931HCID 20228931, 화합물HCID 538470992-Chloro-6-quinoxalinecarbonyl chloride

생성물 1

HCID 86677177HCID 86677177, 화합물수율 24.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of O, N-dimethyl-hydroxylamine hydrochloride salt (29 g, 0.30 mol, 1.1 eq) and DIEA (182 mL, 1.08 mol, 4.0 eq) in DCM (300 mL) was added the mixture of 3-chloro-quinoxaline-6-carbonyl chloride and 2-chloro-quinoxaline-6-carbonyl chloride (52 g, 0.27 mol, 1.0 eq) at 0° C. The mixture was stirred at rt overnight, then concentrated. The resulting residue was washed with water (300 mL×2) and extracted with EA (300 mL×2). The combined organic layers were dried over anhydrous Na2SO4, filtered and concentrated. The resulting solid was triturated with EA/PE =1/1 (300 mL) to afford 3-chloro-N-methoxy-N-methylquinoxaline-6-carboxamide (16.5 g, 24.3%).

후처리

  1. concentrationconcentrated
  2. washThe resulting residue was washed with water (300 mL×2)
  3. extractionextracted with EA (300 mL×2)
  4. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe resulting solid was triturated with EA/PE =1/1 (300 mL)

출처 및 근거

ORD 기록
ord-7dd27f32369a4b31ba39c2fb25a80c79
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09295671B2

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