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

Trifluoroacetic acid → HCID 86708565, 화합물

HRID 1430871
노트
인쇄 미리보기

반응식

HRID 1430871 반응식
[Cl:1][C:2]1[C:7]([N:8]2[CH2:14][CH:13]([F:15])[CH2:12][N:11]([CH:16]3[CH2:19][O:18][CH2:17]3)[CH2:10][CH2:9]2)=[CH:6][C:5]([C:20]#[N:21])=[CH:4][C:3]=1[NH:22][C:23]1[N:28]=[C:27]([N:29]([CH:39]2[CH2:41][CH2:40]2)CC2C=CC(OC)=CC=2)[C:26]2=[N:42][CH:43]=[C:44]([C:45]#[N:46])[N:25]2[N:24]=1.C1(OC)C=CC=CC=1.C(O)(C(F)(F)F)=O>ClCCCl>[Cl:1][C:2]1[C:7]([N:8]2[CH2:14][CH:13]([F:15])[CH2:12][N:11]([CH:16]3[CH2:19][O:18][CH2:17]3)[CH2:10][CH2:9]2)=[CH:6][C:5]([C:20]#[N:21])=[CH:4][C:3]=1[NH:22][C:23]1[N:28]=[C:27]([NH:29][CH:39]2[CH2:40][CH2:41]2)[C:26]2=[N:42][CH:43]=[C:44]([C:45]#[N:46])[N:25]2[N:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acid2회HCID 7519AnisoleHCID 86708566(+/-)2-((2-Chloro-5-cyano-3-(6-fluoro-4-(oxetan-3-yl)-1,4-diazepan-1-yl)phenyl)amino)-4-(cyclopropyl(4-methoxybenzyl)amino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile

생성물 1

HCID 86708565HCID 86708565, 화합물수율 16.7%

시약·촉매·용매 1

HCID 11
1,2-Dichloroethane
용매

실험 절차

(+/−) 2-((2-chloro-5-cyano-3-(6-fluoro-4-(oxetan-3-yl)-1,4-diazepan-1-yl)phenyl)amino)-4-(cyclopropyl(4-methoxybenzyl)amino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (89 mg, 0.138 mmol) was taken up in DCE (1 mL) and anisole (0.076 mL, 0.692 mmol) was added, followed by TFA (0.640 mL, 8.30 mmol). The reaction was stirred at rt overnight. An additional 1 ml of TFA was added, and the reaction was stirred at rt for 4 h. The solvent was removed in vacuo and the material dissolved in MeOH. The material was loaded onto an SCX column (5 g, benzenesulfonic acid sorbent) and the column was flushed with MeOH, then 1:1 DCM/7N NH3/MeOH to obtain the product. The solvent was removed in vacuo and the crude material was purified by preparative HPLC. 2-((2-chloro-5-cyano-3-(6-fluoro-4-(oxetan-3-yl)-1,4-diazepan-1-yl)phenyl)amino)-4-(cyclopropylamino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (12 mg, 0.023 mmol, 16.6% yield) was obtained as a yellow solid.

후처리

  1. stirringthe reaction was stirred at rt for 4 h
  2. customThe solvent was removed in vacuo
  3. dissolutionthe material dissolved in MeOH
  4. customthe column was flushed with MeOH
  5. custom1:1 DCM/7N NH3/MeOH to obtain the product
  6. customThe solvent was removed in vacuo
  7. customthe crude material was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-89dcb950a251443fae3d9990855c07f5
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08940736B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트