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Trifluoroacetic acid → Trifluoroacetic acid

HRID 1662828
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인쇄 미리보기

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HRID 1662828 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([S:14]([C:17]2[CH:22]=[CH:21][C:20]([NH:23][C:24]3[N:29]=[CH:28][C:27]([NH:30][C:31](=[O:50])[C:32]4[CH:37]=[C:36]([NH:38][C:39](=[O:48])[C:40]5[CH:45]=[CH:44][C:43]([O:46][CH3:47])=[CH:42][CH:41]=5)[CH:35]=[CH:34][C:33]=4[Cl:49])=[CH:26][N:25]=3)=[CH:19][CH:18]=2)(=[O:16])=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.[C:51]([OH:57])([C:53]([F:56])([F:55])[F:54])=[O:52]>C(Cl)Cl>[Cl:49][C:33]1[CH:34]=[CH:35][C:36]([NH:38][C:39](=[O:48])[C:40]2[CH:41]=[CH:42][C:43]([O:46][CH3:47])=[CH:44][CH:45]=2)=[CH:37][C:32]=1[C:31]([NH:30][C:27]1[CH:26]=[N:25][C:24]([NH:23][C:20]2[CH:19]=[CH:18][C:17]([S:14]([CH:11]3[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]3)(=[O:15])=[O:16])=[CH:22][CH:21]=2)=[N:29][CH:28]=1)=[O:50].[C:51]([OH:57])([C:53]([F:56])([F:55])[F:54])=[O:52]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acidHCID 596527184-(4-{5-[2-Chloro-5-(4-Methoxy-Benzoylamino)-Benzoylamino]-Pyrimidin-2-ylamino}-Benzenesulfonyl)-Piperidine-1-Carboxylic Acid tert-Butyl Ester

생성물 2

HCID 6422Trifluoroacetic acid수율 99%HCID 249607312-Chloro-5-(4-Methoxy-Benzoylamino)-N-{2-[4-(Piperidine-4-Sulfonyl)-Phenylamino]-Pyrimidin-5-yl}-Benzamide

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

A stirred suspension of intermediate 28 (Example 41) (0.075 g, 0.104 mmol) in DCM (8 mL) was treated with TFA (0.200 mL) and stirred for 18 h. Solvents were then removed yielding desired product as TFA salt (0.064 g, 99%). 1H NMR (DMSO-d6): δ 1.64-1.70 (m, 2H), 2.01-2.04 (m, 2H), 2.86-2.88 (m, 2H), 3.44-3.48 (m, 1H), 3.84 (s, 3H), 7.08 (d, J=8.8 Hz, 2H), 7.56 (d, J=8.9 Hz, 1H), 7.74 (d, J=8.8 Hz, 2H), 7.90 (dd, J=8.7 Hz, J=2.5 Hz, 1H), 7.98 (d, J=8.9 Hz, 2H), 8.05 (d, J=8.8 Hz, 2H), 8.23 (d, J=2.5 Hz, 1H), 8.24 (br s, 1H), 8.68 (br s, 1H), 8.90 (s, 2H), 10.37 (s, 1H), 10.39 (s, 1H), 10.78 (s, 1H).

후처리

  1. customSolvents were then removed

출처 및 근거

ORD 기록
ord-ee319e62a7604135a2810b691dc560f8
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030487B2

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