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Trifluoroacetic acid → HCID 86708565, 화합물

HRID 921693
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HRID 921693 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 16.6%

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 room temperature overnight. An additional 1 ml of TFA was added, and the reaction was stirred at room temperature 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-(cyclopropyl amino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (12 mg) was obtained as a yellow solid.

후처리

  1. stirringthe reaction was stirred at room temperature 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-5823a971d6264b22bfb51d783995b73e
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273057B2

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