Hydrochloric Acid → HCID 50906578, 화합물

HRID 1963051노트

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HRID 1963051 반응식
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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 70663719HCID 70663719, 화합물

생성물 1

HCID 50906578HCID 50906578, 화합물수율 96.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

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:

후처리

  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.

출처 및 근거

ORD 기록
ord-4c338606edba463b925d7188722485bb
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415336B2

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