Hydrochloric Acid → HCID 50906578、化合物

HRID 1963051ノート

反応式

HRID 1963051 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[N:24]3[C:19]([CH:20]=[CH:21][CH:22]=[CH:23]3)=[C:18]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:17]=2[CH2:31][C:32]2[C:37]([F:38])=[CH:36][CH:35]=[CH:34][C:33]=2[Cl:39])=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.O1CCOCC1>C(Cl)Cl>[Cl:39][C:33]1[CH:34]=[CH:35][CH:36]=[C:37]([F:38])[C:32]=1[CH2:31][C:17]1[C:18]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[C:19]2[N:24]([C:16]=1[C:14]([N:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1)=[O:15])[CH:23]=[CH:22][CH:21]=[CH:20]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 70663719HCID 70663719、化合物

生成物 1

HCID 50906578HCID 50906578、化合物収率 96.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

The compound of step 3 (0.886 g, 1.62 mmol) was dissolved in DCM (6.5 ml). The solution was cooled at 0° C. and a 4 N solution of hydrogen chloride in dioxane (2.02 ml, 8.08 mmol) was added. After stirring overnight at room temperature, the mixture was concentrated to dryness. The residue was triturated several times with diethyl ether, filtered, rinsed with diethyl ether and dried in a vacuo at 65° C. to give 0.70 g of the title compound in the form of [2-(2-chloro-6-fluoro-benzyl)-1-phenyl-indolizin-3-yl]-piperazin-1-yl-methanone hydrochloride as an off-white powder with the following characteristics:

後処理

  1. concentrationthe mixture was concentrated to dryness
  2. customThe residue was triturated several times with diethyl ether
  3. filtrationfiltered
  4. washrinsed with diethyl ether
  5. customdried in a vacuo at 65° C.

出典と根拠

ORDレコード
ord-4c338606edba463b925d7188722485bb
出典データセット
uspto-grants-2013_04
特許番号
US08415336B2

反応ノート

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