P-Anisidine → N4-Adamant-1-yl-N6-(4-methoxyphenyl)pyrimidine-4,6-diamine

HRID 876157

反応式

HRID 876157 の反応式
[C:1]12([NH:11][C:12]3[CH:17]=[C:16](Cl)[N:15]=[CH:14][N:13]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.[CH3:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([NH2:27])=[CH:23][CH:22]=1.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1>C1(C)C=CC=CC=1.CC([O-])=O.CC([O-])=O.[Pd+2]>[C:1]12([NH:11][C:12]3[CH:17]=[C:16]([NH:27][C:24]4[CH:25]=[CH:26][C:21]([O:20][CH3:19])=[CH:22][CH:23]=4)[N:15]=[CH:14][N:13]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2

参加物

6

反応物 3

HCID 7732P-AnisidineHCID 634876Binap, (A+-)-HCID 534860716-chloro-N-(1-Adamantyl)pyrimidin-4-amine

生成物 1

HCID 70941076N4-Adamant-1-yl-N6-(4-methoxyphenyl)pyrimidine-4,6-diamine収率 65%

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 1140Toluene溶媒

実験手順

100 mg of N-adamant-1-yl-6-chloropyrimidin-4-amine, 56 mg of p-anisidine, 73 mg of Na-butylate, 2.2 mg of Pd(OAc)2 and 12 mg of BINAP were taken in a screw cap vial under agron in 4 mL of dry toluene and the vial was kept in a heating block at 150° C. for 12 hours. The mixture obtained was cooled to r.t. and purification was carried out by column chromatography using PE:EtOAc 2:1. N4-Adamant-1-yl-N6-(4-methoxyphenyl)pyrimidine-4,6-diamine was obtained.

後処理

  1. customThe mixture obtained
  2. custompurification

出典と根拠

ORDレコード
ord-c8eea45fbae14fdb81a3532519effe2e
出典データセット
uspto-grants-2015_03
特許番号
US08986994B2

関連ノート

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