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Hydrochloric Acid → 2-(3-Fluoro-2-methyl-benzyl)-1-phenyl-3-(piperazine-1-carbonyl)-indolizine-7-carboxylic acid methylamide

HRID 1963059
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인쇄 미리보기

반응식

HRID 1963059 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[N:24]3[C:19]([CH:20]=[C:21]([C:25](=[O:28])[NH:26][CH3:27])[CH:22]=[CH:23]3)=[C:18]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:17]=2[CH2:35][C:36]2[CH:41]=[CH:40][CH:39]=[C:38]([F:42])[C:37]=2[CH3:43])=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.O1CCOCC1>C(Cl)Cl>[CH3:27][NH:26][C:25]([C:21]1[CH:22]=[CH:23][N:24]2[C:19]([CH:20]=1)=[C:18]([C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[C:17]([CH2:35][C:36]1[CH:41]=[CH:40][CH:39]=[C:38]([F:42])[C:37]=1[CH3:43])=[C:16]2[C:14]([N:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)=[O:15])=[O:28]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 677721744-[2-(3-Fluoro-2-methyl-benzyl)-7-methylcarbamoyl-1-phenyl-indolizine-3-carbonyl]-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 509065792-(3-Fluoro-2-methyl-benzyl)-1-phenyl-3-(piperazine-1-carbonyl)-indolizine-7-carboxylic acid methylamide수율 99.4%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

반응 조건

온도
0 °C

실험 절차

The compound of step 7 (0.065 g, 0.11 mmol) was dissolved in 1.1 ml of DCM and cooled to 0° C. and a 4 N solution of hydrogen chloride in dioxane (0.54 ml, 2.20 mmol) was added. The mixture was stirred at room temperature overnight and then evaporated to dryness under reduced pressure. The obtained solid was triturated several times with diethyl ether and dried in vacuo at 40° C. 0.053 g of the title compound were obtained in the form of 2-(3-fluoro-2-methyl-benzyl)-1-phenyl-3-(piperazine-1-carbonyl)-indolizine-7-carboxylic acid methylamide hydrochloride as a light yellow solid with the following characteristics:

후처리

  1. customevaporated to dryness under reduced pressure
  2. customThe obtained solid was triturated several times with diethyl ether
  3. customdried in vacuo at 40° C

출처 및 근거

ORD 기록
ord-0ff3118ba2c0402f8f345a3ecc0bcb20
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415336B2

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