4-Hydroxyxylidine → N2,N4-bis-(2,3-dimethyl-4-hydroxyphenyl)-5-fluoro-2,4-pyrimidinediamine

HRID 76495

反応式

HRID 76495 の反応式
Cl[C:2]1[N:7]=[C:6](Cl)[C:5]([F:9])=[CH:4][N:3]=1.[CH3:10][C:11]1[C:17]([CH3:18])=[C:16]([OH:19])[CH:15]=[CH:14][C:12]=1[NH2:13]>>[CH3:10][C:11]1[C:17]([CH3:18])=[C:16]([OH:19])[CH:15]=[CH:14][C:12]=1[NH:13][C:2]1[N:7]=[C:6]([NH:13][C:12]2[CH:14]=[CH:15][C:16]([OH:19])=[C:17]([CH3:18])[C:11]=2[CH3:10])[C:5]([F:9])=[CH:4][N:3]=1

参加物

3

反応物 2

HCID 765424-HydroxyxylidineHCID 2507052,4-Dichloro-5-fluoropyrimidine

生成物 1

HCID 22060616N2,N4-bis-(2,3-dimethyl-4-hydroxyphenyl)-5-fluoro-2,4-pyrimidinediamine

実験手順

In like manner to the preparation of N2,N4-bis(3-hydroxyphenyl)-5-fluoro-2,4-pyrimidinediamine, the reaction of 2,4-dichloro-5-fluoropyrimidine with 2,3-dimethyl-4-hydroxyaniline gave N2,N4-bis-(2,3-dimethyl-4-hydroxyphenyl)-5-fluoro-2,4-pyrimidinediamine. LCMS: ret. time: 19.07 min.; purity: 99%; MS (m/e): 369 (MH+); 1H NMR (DMSO-d6): δ 9.21 (1H, s), 8.99 (1H, s), 8.63 (1H, s), 7.92 (1H, s), 7.84 (1H, d, J=3.6 Hz), 6.94 (1H, d, J=8.5 Hz), 6.85 (1H, d, J=8.5 Hz), 6.70 (1H, d, J=8.5 Hz), 6.58 (1H, d, J=8.5 Hz), 2.12 (3H, s), 2.06 (3H, s), 2.02 (3H, s), 1.94 (3H, s).

後処理

  1. customIn like manner to the preparation of N2,N4-bis(3-hydroxyphenyl)-5-fluoro-2,4-pyrimidinediamine

出典と根拠

ORDレコード
ord-26b185a02ccf40c38d305f902d76d735
出典データセット
uspto-grants-2014_09
特許番号
US08835430B2

関連ノート

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