Trifluoroacetic acid → Trifluoroacetic acid

HRID 1662826ノート

反応式

HRID 1662826 の反応式
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]([C:46]#[N: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]([C:46]#[N: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[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]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]

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 674282094-(4-{5-[2-Chloro-5-(4-Cyano-Benzoylamino)-Benzoylamino]-Pyrimidin-2-ylamino}-Benzenesulfonyl)-Piperidine-1-Carboxylic Acid tert-Butyl Ester

生成物 2

HCID 6422Trifluoroacetic acid収率 99%HCID 249603692-Chloro-5-(4-Cyano-Benzoylamino)-N-{2-[4-(Piperidine-4-Sulfonyl)-Phenylamino]-Pyrimidin-5-yl}-Benzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A stirred suspension of intermediate 27 (Example 39) (0.12 g, 0.143 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 (0.104 g, 99%). 1H NMR (DMSO-d6): δ 1.61-1.70 (m, 2H), 2.01-2.04 (m, 2H), 2.80-2.90 (m, 2H), 7.61 (d, J=8.8 Hz, 1H), 7.74 (d, J=8.9 Hz, 2H), 7.90 (dd, J=8.7 Hz, J=2.5 Hz, 1H), 8.04-8.13 (m, 7H), 8.21-8.25 (m, 1H), 8.64-8.68 (m, 1H), 8.90 (s, 2H), 10.37 (s, 1H), 10.78 (s, 1H), 10.80 (s, 1H).

後処理

  1. customSolvents were then removed

出典と根拠

ORDレコード
ord-96829ca63ea749a7a0a839a07cac586d
出典データセット
uspto-grants-2011_10
特許番号
US08030487B2

反応ノート

読み込み中…