홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

2-chloro-N,N-dimethylacetamide → HCID 70945201, 화합물

HRID 517976
노트
인쇄 미리보기

반응식

HRID 517976 반응식
FC(F)(F)C(O)=O.[CH3:8][N:9]1[C:17]2[CH:16]=[C:15]([C:18]3[CH:19]=[N:20][C:21]([O:28][CH2:29][CH2:30][CH:31]4[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]4)=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=3)[N:14]=[C:13]([C:37]#[N:38])[C:12]=2[N:11]=[N:10]1.C(N(CC)C(C)C)(C)C.[Cl:48][CH2:49][C:50]([N:52]([CH3:54])[CH3:53])=[O:51]>C(#N)C>[ClH:48].[CH3:8][N:9]1[C:17]2[CH:16]=[C:15]([C:18]3[CH:19]=[N:20][C:21]([O:28][CH2:29][CH2:30][CH:31]4[CH2:36][CH2:35][N:34]([CH2:49][C:50]([N:52]([CH3:54])[CH3:53])=[O:51])[CH2:33][CH2:32]4)=[C:22]([C:24]([F:25])([F:26])[F:27])[CH:23]=3)[N:14]=[C:13]([C:37]#[N:38])[C:12]=2[N:11]=[N:10]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 758862-chloro-N,N-dimethylacetamideHCID 81531DiisopropylethylamineHCID 866733511-methyl-6-(6-(2-(piperidin-4-yl)ethoxy)-5-(trifluoromethyl)pyridin-3-yl)-1H-[1,2,3]triazolo[4,5-c]pyridine-4-carbonitrile trifluoroacetate

생성물 1

HCID 70945201HCID 70945201, 화합물수율 88.3%

시약·촉매·용매 1

HCID 6342Acetonitrile
용매

반응 조건

온도
20 °C

실험 절차

To a solution of 1-methyl-6-(6-(2-(piperidin-4-yl)ethoxy)-5-(trifluoromethyl)-pyridin-3-yl)-1H-[1,2,3]triazolo[4,5-c]pyridine-4-carbonitrile trifluoroacetate (200 mg) and N,N-diisopropylethylamine (310 μl) in acetonitrile (8 ml), 2-chloro-N,N-dimethylacetamide (77 μl, 91 mg) was added and the mixture stirred at 20° C. for 65 h. The reaction mixture was concentrated. The residue diluted with water (20 ml) and extrated with DCM (50 ml×3), combined DCM layer dried over sodium sulphate and solvent removed under reduced pressure. The residue was then purified by Strata Si column (5 g, dichloromethane:methanol=1:0, 25:1 to 15:1), converted to hydrochloric acid salt using 2N hydrochloric acid in diethyl ether to give 1-methyl-6-(6-(2-(1-(2-dimethylamino-2-oxo-ethyl)piperidin-4-yl)ethoxy)-5-(trifluoromethyl)pyridin-3-yl)-1H-[1,2,3]triazolo[4,5-c]pyridine-4-carbonitrile hydrochloride (179 mg).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additionThe residue diluted with water (20 ml)
  3. dry with materialdried over sodium sulphate and solvent
  4. customremoved under reduced pressure
  5. customThe residue was then purified by Strata Si column (5 g, dichloromethane:methanol=1:0, 25:1 to 15:1)

출처 및 근거

ORD 기록
ord-e04a2a945f564b1db4571999ca5d01d3
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115126B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트