1,2-Dichloroethane → HCID 86637004、化合物

HRID 1366607ノート

反応式

HRID 1366607 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([N:8]([CH3:15])[CH2:9][C:10]2[S:11][CH:12]=[CH:13][N:14]=2)[C:5]([F:16])=[C:4]([NH:17][NH2:18])[N:3]=1.[CH:19]1([CH2:24][C@H:25]([CH2:29][N:30]([CH:38]=[O:39])[O:31][CH:32]2[CH2:37][CH2:36][CH2:35][CH2:34][O:33]2)[C:26](O)=[O:27])[CH2:23][CH2:22][CH2:21][CH2:20]1.CN1CCOCC1.C1C=NC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C=O)C>[Cl:1][C:2]1[N:3]=[C:4]([NH:17][NH:18][C:26](=[O:27])[C@H:25]([CH2:24][CH:19]2[CH2:20][CH2:21][CH2:22][CH2:23]2)[CH2:29][N:30]([O:31][CH:32]2[CH2:37][CH2:36][CH2:35][CH2:34][O:33]2)[CH:38]=[O:39])[C:5]([F:16])=[C:6]([N:8]([CH3:15])[CH2:9][C:10]2[S:11][CH:12]=[CH:13][N:14]=2)[N:7]=1

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 181649HOAtHCID 57937086(2R)-3-cyclopentyl-2-{[formyl(tetrahydro-2H-pyran-2-yloxy)amino]methyl}propanoic acidHCID 866370032-chloro-5-fluoro-6-hydrazino-N-methyl-N-(1,3-thiazol-2-ylmethyl)-4-pyrimidinamine

生成物 1

HCID 86637004HCID 86637004、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-Chloro-5-fluoro-6-hydrazino-N-methyl-N-(1,3-thiazol-2-ylmethyl)-4-pyrimidinamine (assumed dihydrochloride) (0.9034 g, 2.509 mmol) and (2R)-3-cyclopentyl-2-{[formyl(tetrahydro-2H-pyran-2-yloxy)amino]methyl}propanoic acid (1.299 g, 3.01 mmol) were dissolved in DMF (13 mL). NMM (1.655 mL, 15.05 mmol) was added, followed by HOAt (0.4095 g, 3.01 mmol) and EDC (0.577 g, 3.01 mmol). After stirring overnight, the reaction mixture was purified by RP-HPLC to provide [(2R)-3-(2-{2-chloro-5-fluoro-6-[methyl(1,3-thiazol-2-ylmethyl)amino]-4-pyrimidinyl}hydrazino)-2-(cyclopentylmethyl)-3-oxopropyl](tetrahydro-2H-pyran-2-yloxy)formamide as a red sticky material. LCMS: (M+H)+=570.2.

後処理

  1. customthe reaction mixture was purified by RP-HPLC

出典と根拠

ORDレコード
ord-5b832b8be6e345ee9fc4978059eb7142
出典データセット
uspto-grants-2011_02
特許番号
US07893056B2

反応ノート

読み込み中…