Hydrochloric Acid → 2-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide hydrochloride

HRID 2408901노트

반응식

HRID 2408901 반응식
Cl.[NH2:2][C:3]1[C:4]2[C:5]3[C:6](=[N:18][N:19]([CH2:21][C:22]4[C:27]([Cl:28])=[C:26]([O:29][CH3:30])[C:25]([CH3:31])=[CH:24][N:23]=4)[N:20]=2)[CH:7]=[C:8]([CH2:13][C:14]([NH:16][CH3:17])=[O:15])[C:9]=3[CH2:10][S:11][N:12]=1>C(O)C>[ClH:28].[NH2:2][C:3]1[C:4]2[C:5]3[C:6](=[N:18][N:19]([CH2:21][C:22]4[C:27]([Cl:28])=[C:26]([O:29][CH3:30])[C:25]([CH3:31])=[CH:24][N:23]=4)[N:20]=2)[CH:7]=[C:8]([CH2:13][C:14]([NH:16][CH3:17])=[O:15])[C:9]=3[CH2:10][S:11][N:12]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 666180742-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide

생성물 1

HCID 666180732-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide hydrochloride수율 194.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3 M hydrochloric acid (9.2 ml, 27.8 mmol) was added dropwise to an ethanol (200 ml) suspension of 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (5446.6 mg, 11.6 mmol) at 25° C., while the suspension was stirred. The resulting mixture was stirred for 3.5 hours. The obtained crystal was collected by filtration, was then washed with ethanol (50 ml), and was then dried under reduced pressure at 40° C. for 14 hours, so as to obtain the above title compound (5436.1 mg, 116. mmol). Yield: 99%.

후처리

  1. stirringThe resulting mixture was stirred for 3.5 hours
  2. filtrationThe obtained crystal was collected by filtration
  3. washwas then washed with ethanol (50 ml)
  4. customwas then dried under reduced pressure at 40° C. for 14 hours

출처 및 근거

ORD 기록
ord-670d00eeee6f4f4b8a37dda5572fbe26
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08815880B2

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