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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → HCID 57519920, 화합물

HRID 1528097
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HRID 1528097 반응식
ClC(O[C:6](=[O:12])OC(Cl)(Cl)Cl)(Cl)Cl.[F:13][C:14]([F:23])([F:22])[C:15]1[N:20]=[C:19]([NH2:21])[CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C.[Br:31][C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[N:38]=[CH:37][CH:36]=[C:35]2[NH2:42]>C(Cl)Cl>[Br:31][C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[N:38]=[CH:37][CH:36]=[C:35]2[NH:42][C:6]([NH:21][C:19]1[CH:18]=[CH:17][CH:16]=[C:15]([C:14]([F:13])([F:22])[F:23])[N:20]=1)=[O:12]
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참가 물질

6

반응물 4

HCID 8471Triethylamine2회HCID 94429TriphosgeneHCID 8210242-Amino-6-(trifluoromethyl)pyridineHCID 27563746-Bromoquinolin-4-amine

생성물 1

HCID 57519920HCID 57519920, 화합물수율 159.6%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매
2회

반응 조건

온도
0 °C

실험 절차

366 mg of bis(trichloromethyl)carbonate (1.234 mmol) were dissolved in 7 ml of DCM and cooled to 0° C. To this mixture the solution of 400 mg of 6-(trifluoromethyl)pyridin-2-amine (2.467 mmol) and 379 μl of triethylamine (5.43 mmol) in 9.7 ml DCM was slowly added over 60 minutes at 0° C., and stirring was continued for an additional 60 minutes at room temperature. 550 mg of 6-bromoquinolin-4-amine (2.467 mmol) and 379 μl of triethylamine (5.43 mmol) were suspended in 9.7 ml and subsequently slowly added to the reaction mixture at RT, which became a clear solution after 45 minutes. After stirring over night the reaction mixture was poured into ice water and stirred for 2 h. The precipitation formed was filtered off and dried in vacuum for 24 h. 810 mg of the desired product were obtained as an off white powder (yield: 80%). The quite pure raw material was used without further purification in the next step.

후처리

  1. additionsubsequently slowly added to the reaction mixture at RT
  2. customafter 45 minutes
  3. stirringAfter stirring over night the reaction mixture
  4. stirringstirred for 2 h
  5. customThe precipitation
  6. customformed
  7. filtrationwas filtered off
  8. customdried in vacuum for 24 h

출처 및 근거

ORD 기록
ord-75cbc8e726af4a1ca4d5fc7b3a9538d9
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09090592B2

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