Trifluoroacetic acid → N-(3-(2-Fluorobenzyl)-3-(methoxymethyl)piperidin-1-yl)-3-(2-methylpyridin-4-yl)-1H-indazole-5-carboxamide

HRID 530888ノート

反応式

HRID 530888 の反応式
[F:1][C:2]1[CH:55]=[CH:54][CH:53]=[CH:52][C:3]=1[CH2:4][C:5]1([CH2:49][O:50][CH3:51])[CH2:10][CH2:9][CH2:8][N:7]([NH:11][C:12]([C:14]2[CH:15]=[C:16]3[C:20](=[CH:21][CH:22]=2)[N:19](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[N:18]=[C:17]3[C:42]2[CH:47]=[CH:46][N:45]=[C:44]([CH3:48])[CH:43]=2)=[O:13])[CH2:6]1.FC(F)(F)C(O)=O.C([SiH](CC)CC)C>>[F:1][C:2]1[CH:55]=[CH:54][CH:53]=[CH:52][C:3]=1[CH2:4][C:5]1([CH2:49][O:50][CH3:51])[CH2:10][CH2:9][CH2:8][N:7]([NH:11][C:12]([C:14]2[CH:15]=[C:16]3[C:20](=[CH:21][CH:22]=2)[NH:19][N:18]=[C:17]3[C:42]2[CH:47]=[CH:46][N:45]=[C:44]([CH3:48])[CH:43]=2)=[O:13])[CH2:6]1

参加物

4

反応物 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 68074196N-(3-(2-Fluorobenzyl)-3-(methoxymethyl)piperidin-1-yl)-3-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxamide

生成物 1

HCID 67985892N-(3-(2-Fluorobenzyl)-3-(methoxymethyl)piperidin-1-yl)-3-(2-methylpyridin-4-yl)-1H-indazole-5-carboxamide

実験手順

In a flask, N-(3-(2-fluorobenzyl)-3-(methoxymethyl)piperidin-1-yl)-3-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxamide (crude, from previous step) was reacted with trifluoroacetic acid (3 mL) for 1 hour. After reaction completion triethylsilane (0.1 mL) was added, and the reaction was stirred for an additional 15 minutes. The reaction was concentrated and rinsed with diethyl ether. The resulting remaining precipitate was dried and further purified using HPLC to give the titled compound. LC-MS: 488.24 [M+H]. LC/MS RT=2.49 min.

後処理

  1. additionwas added
  2. concentrationThe reaction was concentrated
  3. washrinsed with diethyl ether
  4. customThe resulting remaining precipitate was dried
  5. customfurther purified

出典と根拠

ORDレコード
ord-40c27145af0f46938c98a5616f52a313
出典データセット
uspto-grants-2016_05
特許番号
US09351965B2

反応ノート

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