Hydrochloric Acid → 3-(2-bromo-6-fluoro-phenyl)-1-methyl-7-(4-methyl-1,1-dioxo-1,2,3,4-tetrahydro-1lambda*6*-benzo[1,4]thiazin-7-ylamino)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one

HRID 9733ノート

反応式

HRID 9733 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[CH2:18][C:17]2[C:12](=[N:13][C:14](S(C)(=O)=O)=[N:15][CH:16]=2)[N:11]([CH3:23])[C:10]1=[O:24].[NH2:25][C:26]1[CH:38]=[CH:37][C:29]2[N:30]([CH3:36])[CH:31]=[CH:32][S:33](=[O:35])(=[O:34])[C:28]=2[CH:27]=1.Cl>CN1C(=O)CCC1.CCOCC>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[CH2:18][C:17]2[C:12](=[N:13][C:14]([NH:25][C:26]3[CH:38]=[CH:37][C:29]4[N:30]([CH3:36])[CH2:31][CH2:32][S:33](=[O:35])(=[O:34])[C:28]=4[CH:27]=3)=[N:15][CH:16]=2)[N:11]([CH3:23])[C:10]1=[O:24]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 219881503-(2-Bromo-6-fluorophenyl)-3,4-dihydro-7-methanesulphonyl-1-methylpyrimido[4,5-d]pyrimidin-2(1h)-oneHCID 219881597-Amino-4-methyl-4h-benzo[1,4]thiazin-1,1-dioxide2 回

生成物 1

HCID 100076313-(2-bromo-6-fluoro-phenyl)-1-methyl-7-(4-methyl-1,1-dioxo-1,2,3,4-tetrahydro-1lambda*6*-benzo[1,4]thiazin-7-ylamino)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one収率 31.1%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
120 °C

実験手順

83 mg 3-(2-bromo-6-fluorophenyl)-3,4-dihydro-7-methanesulphonyl-1-methyl-pyrimido[4,5-d]pyrimidin-2(1H)-one and 85 mg 7-Amino-4-methyl-4H-benzo[1,4]thiazin-1,1-dioxide (starting material n)) in 0.8 ml NMP were treated with 0.2 ml 2M HCl in ether and heated to 120° C. for 6 hrs. The mixture was purified by preparative HPLC-MS to yield 34 mg of the title compound.

後処理

  1. customThe mixture was purified by preparative HPLC-MS

出典と根拠

ORDレコード
ord-29b0fbe5e63c4c83a1b1bf1aabfd45bd
出典データセット
uspto-grants-2006_08
特許番号
US07091345B2

反応ノート

読み込み中…