O-Methylhydroxylamine hydrochloride → HCID 87222433、化合物

HRID 712275ノート

反応式

HRID 712275 の反応式
Cl.[CH3:2][O:3][NH2:4].[C:5]([C:8]1[C:16]2[S:15][C:14]([NH:17][C:18](=[O:22])[NH:19][CH2:20][CH3:21])=[N:13][C:12]=2[CH:11]=[C:10]([C:23]2[CH:24]=[N:25][C:26]([N:29]3[CH2:34][CH2:33][C:32]([CH3:40])([C:35]([O:37][CH2:38][CH3:39])=[O:36])[CH2:31][CH2:30]3)=[N:27][CH:28]=2)[CH:9]=1)(=O)[CH3:6]>CN(C=O)C>[CH2:20]([NH:19][C:18]([NH:17][C:14]1[S:15][C:16]2[C:8](/[C:5](/[CH3:6])=[N:4]/[O:3][CH3:2])=[CH:9][C:10]([C:23]3[CH:28]=[N:27][C:26]([N:29]4[CH2:30][CH2:31][C:32]([CH3:40])([C:35]([O:37][CH2:38][CH3:39])=[O:36])[CH2:33][CH2:34]4)=[N:25][CH:24]=3)=[CH:11][C:12]=2[N:13]=1)=[O:22])[CH3:21]

参加物

4

反応物 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 86663987Ethyl 1-[5-[7-acetyl-2-(ethylcarbamoylamino)-1,3-benzothiazol-5-yl]pyrimidin-2-yl]-4-methyl-piperidine-4-carboxylate

生成物 1

HCID 87222433HCID 87222433、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

O-Methyl hydroxylamine hydrochloride (64 mg, 0.784 mmol) was added to ethyl 1-[5-[7-acetyl-2-(ethylcarbamoylamino)-1,3-benzothiazol-5-yl]pyrimidin-2-yl]-4-methyl-piperidine-4-carboxylate (200 mg, 0.39 mmol) in DMF (5 mL). The reaction mixture was heated to 60° C. for 4 h after which time LCMS indicated clean conversion to the desired product. The reaction was diluted with EtOAc, washed with water then brine and the organic layer dried (MgSO4), filtered and the solvent removed in vacuo. The crude product obtained was used in the next step.

出典と根拠

ORDレコード
ord-11fe1b5aad664f1382a5c5a780db6bbe
出典データセット
uspto-grants-2015_11
特許番号
US09181234B2

反応ノート

読み込み中…