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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Trifluoroacetic acid → Trifluoroacetic acid

HRID 711521
ノート
印刷プレビュー

反応式

HRID 711521 の反応式
[F:1][CH:2]([F:45])[N:3]1[CH:7]=[C:6]([C:8]2[C:13]3[C:14](=[O:28])[N:15](CC4C=CC(OC)=CC=4OC)[CH2:16][C:12]=3[C:11]([F:29])=[C:10]([NH:30][C@@H:31]3[CH2:36][CH2:35][CH2:34][CH2:33][C@@H:32]3[NH:37]C(=O)OC(C)(C)C)[N:9]=2)[CH:5]=[N:4]1.[C:46]([OH:52])([C:48]([F:51])([F:50])[F:49])=[O:47]>>[NH2:37][C@H:32]1[CH2:33][CH2:34][CH2:35][CH2:36][C@H:31]1[NH:30][C:10]1[N:9]=[C:8]([C:6]2[CH:5]=[N:4][N:3]([CH:2]([F:1])[F:45])[CH:7]=2)[C:13]2[C:14](=[O:28])[NH:15][CH2:16][C:12]=2[C:11]=1[F:29].[C:46]([OH:52])([C:48]([F:51])([F:50])[F:49])=[O:47]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86654725tert-Butyl (1S,2R)-2-(4-(1-(difluoromethyl)-1H-pyrazol-4-yl)-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)cyclohexylcarbamate

生成物 2

HCID 6422Trifluoroacetic acid収率 86%HCID 532503696-((1R,2S)-2-Aminocyclohexylamino)-4-(1-(difluoromethyl)-1H-pyrazol-4-yl)-7-fluoro-1H-pyrrolo[3,4-c]pyridin-3(2H)-one

実験手順

A solution of tert-butyl (1S,2R)-2-(4-(1-(difluoromethyl)-1H-pyrazol-4-yl)-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)cyclohexylcarbamate (36 mg, 0.057 mmol) in TFA (2 mL) was heated at 60° C. for 2 h. After removal of the solvent, the residue was diluted in MeOH (2 mL) and was purified by preparative HPLC. The fractions were collected and stripped to dryness via rotary evaporation to yield the title compound as a TFA salt (18.7 mg, 86%). 1H NMR (500 MHz, DMSO-d6) δ ppm 1.40-1.52 (m, 2H), 1.58-1.76 (m, 3H), 1.75-1.94 (m, 3H), 3.67 (br s, 1H), 4.44 (d, J=4.88 Hz, 2H), 4.53 (br s, 1H), 6.86 (d, J=6.83 Hz, 1H), 7.71 (br s, 2H), 7.79-8.12 (m, 1H), 8.53 (s, 2H), 9.41 (s, 1H). [M+H] calc'd for C17H19F3N6O, 381. found, 381.

後処理

  1. customAfter removal of the solvent
  2. additionthe residue was diluted in MeOH (2 mL)
  3. customwas purified by preparative HPLC
  4. customThe fractions were collected
  5. customstripped to dryness via rotary evaporation

出典と根拠

ORDレコード
ord-7960c56cd9144577ab684f732668a3e8
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181255B2

反応ノート

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