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Triethylamine hydrochloride → HCID 23118009, 화합물

HRID 1180713
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HRID 1180713 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]=[C:10](Cl)[C:11]([F:14])([F:13])[F:12].[N-:16]=[N+:17]=[N-:18].[Na+].Cl.C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[C:10]([C:11]([F:14])([F:13])[F:12])=[N:18][N:17]=[N:16]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11130Triethylamine hydrochlorideHCID 33557Sodium AzideHCID 10444178HCID 10444178, 화합물

생성물 1

HCID 23118009HCID 23118009, 화합물수율 97.8%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Four grams (16.8 mmol) of N-(2-methoxyphenyl)-2,2,2-trifluoroacetimidoyl chloride obtained in Example 9, 1.98 g (30.2 mmol) of sodium azide, 1.16 g (8.42 mmol) of triethylamine hydrochloride, and 40 ml of toluene were introduced into a 100 ml flask and reacted at 80° C. for 14 hours. After the reaction, the reaction solution was cooled to room temperature and washed with water (30 ml×2). The organic phase was dried over anhydrous magnesium sulfate for 1 hour, filtered, and then subjected to solvent removal by evaporation. The crude product thus obtained was purified by column chromatography (silica gel, ethyl acetate:hexane=3:7), resulting in 4.01 g of 1-(2-methoxyphenyl)-5-(trifluoromethyl)-1H-tetrazole as a pale yellow oil (yield: 97.6%).

후처리

  1. customreacted at 80° C. for 14 hours
  2. customAfter the reaction
  3. washwashed with water (30 ml×2)
  4. dry with materialThe organic phase was dried over anhydrous magnesium sulfate for 1 hour
  5. filtrationfiltered
  6. customsubjected to solvent removal by evaporation
  7. customThe crude product thus obtained
  8. customwas purified by column chromatography (silica gel, ethyl acetate:hexane=3:7)

출처 및 근거

ORD 기록
ord-db05ce80b84940e08a2a9be7f855aec2
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07282609B2

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