HCID 23002992、化合物 → HCID 66618157、化合物

HRID 2093556ノート

反応式

HRID 2093556 の反応式
[BrH:1].C(O)C.[NH2:5][C:6]1[C:7]2[C:8]3[C:9](=[N:21][N:22]([CH2:24][C:25]4[C:30]([Cl:31])=[C:29]([O:32][CH3:33])[C:28]([CH3:34])=[CH:27][N:26]=4)[N:23]=2)[CH:10]=[C:11]([CH2:16][C:17]([NH:19][CH3:20])=[O:18])[C:12]=3[CH2:13][S:14][N:15]=1>C(#N)C>[BrH:1].[NH2:5][C:6]1[C:7]2[C:8]3[C:9](=[N:21][N:22]([CH2:24][C:25]4[C:30]([Cl:31])=[C:29]([O:32][CH3:33])[C:28]([CH3:34])=[CH:27][N:26]=4)[N:23]=2)[CH:10]=[C:11]([CH2:16][C:17]([NH:19][CH3:20])=[O:18])[C:12]=3[CH2:13][S:14][N:15]=1

参加物

4

反応物 2

HCID 23002992HCID 23002992、化合物HCID 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 66618157HCID 66618157、化合物収率 48.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A 20% hydrobromic acid-ethanol solution (204 μl, 0.505 mmol) was added to an acetonitrile solution (350 ml) 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 (250 mg, 0.561 mmol) at room temperature. The resulting mixture was stirred for 3 hours, and the precipitated solid was then collected by filtration. Ethanol (3 ml) was added to the resulting solid, and the resulting mixture was then stirred for 1 day. Thereafter, the solid was collected by filtration. The solid was then dried under reduced pressure at room temperature for 2 days, so as to obtain the title compound (128 mg, 0.243 mmol).

後処理

  1. filtrationthe precipitated solid was then collected by filtration
  2. additionEthanol (3 ml) was added to the resulting solid
  3. stirringthe resulting mixture was then stirred for 1 day
  4. filtrationThereafter, the solid was collected by filtration
  5. customThe solid was then dried under reduced pressure at room temperature for 2 days

出典と根拠

ORDレコード
ord-de7fd8c92dc3472cb3586667fb2f7e6e
出典データセット
uspto-grants-2013_05
特許番号
US08445504B2

反応ノート

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