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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → HCID 178527452, 화합물

HRID 631866
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HRID 631866 반응식
C([Sn](Cl)(CCCC)CCCC)CCC.[N-:15]=[N+:16]=[N-:17].[Na+].[C:19]([C:21]1[C:30]2[CH2:29][CH2:28][CH2:27][CH2:26][C:25]=2[CH:24]=[CH:23][C:22]=1[NH:31][S:32]([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)(=[O:34])=[O:33])#[N:20].Cl>CN(C=O)C.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[NH:15]1[C:19]([C:21]2[C:30]3[CH2:29][CH2:28][CH2:27][CH2:26][C:25]=3[CH:24]=[CH:23][C:22]=2[NH:31][S:32]([C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)(=[O:34])=[O:33])=[N:20][N:17]=[N:16]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 15096Tributyltin ChlorideHCID 33557Sodium AzideHCID 68296403HCID 68296403, 화합물2회

생성물 1

HCID 178527452HCID 178527452, 화합물수율 5%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide
촉매
HCID 6228Dimethylformamide용매

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온도
220 °C

실험 절차

Tri-n-butyl tin chloride (0.16 mL) was added to a solution of sodium azide (0.039 g) in DMF (0.6 mL) and the mixture was stirred for 5 minutes. Tetra-butyl ammonium bromide (0.0065 g) was then added, followed by N-(1-cyano-5,6,7,8-tetrahydronaphthalen-2-yl)benzenesulfonamide (Intermediate 1, 0.177 g). The mixture was heated by microwave irradiation at 220° C. for 1 hour. The solution was then acidified with 1N hydrochloric acid and the products were extracted into DCM, dried with magnesium sulfate and filtered. The filtrate was evaporated to dryness and the residue was purified by preparative HPLC (C18). The fractions containing the desired product were combined, and the solvent was removed by evaporation to give the title compound as a beige solid (0.01 g).

후처리

  1. extractionthe products were extracted into DCM
  2. dry with materialdried with magnesium sulfate
  3. filtrationfiltered
  4. customThe filtrate was evaporated to dryness
  5. customthe residue was purified by preparative HPLC (C18)
  6. additionThe fractions containing the desired product
  7. customthe solvent was removed by evaporation

출처 및 근거

ORD 기록
ord-c9e28d41af594154b24334a6db0551f5
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321740B2

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