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 2408901ノート

反応式

HRID 2408901 の反応式
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

参加物

4

反応物 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

生成物 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 hydrochloride収率 194.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-670d00eeee6f4f4b8a37dda5572fbe26
出典データセット
uspto-grants-2014_08
特許番号
US08815880B2

反応ノート

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