Water → N-(3-hydroxypropyl)-6-[4-[3-(isopropylamino)-2-pyridyl]piperazine-1-carbonyl]pyridine-3-carboxamide

HRID 381352ノート

反応式

HRID 381352 の反応式
CO[C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7]([C:10]([N:12]2[CH2:17][CH2:16][N:15]([C:18]3[C:23]([NH:24][CH:25]([CH3:27])[CH3:26])=[CH:22][CH:21]=[CH:20][N:19]=3)[CH2:14][CH2:13]2)=[O:11])=[N:6][CH:5]=1.[NH2:29][CH2:30][CH2:31][CH2:32][OH:33].O>CO>[OH:33][CH2:32][CH2:31][CH2:30][NH:29][C:3]([C:4]1[CH:9]=[CH:8][C:7]([C:10]([N:12]2[CH2:13][CH2:14][N:15]([C:18]3[C:23]([NH:24][CH:25]([CH3:27])[CH3:26])=[CH:22][CH:21]=[CH:20][N:19]=3)[CH2:16][CH2:17]2)=[O:11])=[N:6][CH:5]=1)=[O:28]

参加物

5

反応物 3

HCID 962WaterHCID 90863-Amino-1-propanolHCID 109378486-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]nicotinic acid methyl ester

生成物 1

HCID 499740N-(3-hydroxypropyl)-6-[4-[3-(isopropylamino)-2-pyridyl]piperazine-1-carbonyl]pyridine-3-carboxamide収率 78%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

6-[1-[3-(Isopropylamino)-2-pyridyl]piperazine-4-yl-carbonyl]nicotinic acid methyl ester (2.5 g) was dissolved in methanol (40 ml) and with the addition of 3-amino-1-propanol (0.95 g), the mixture was heated to reflux for 12 hours and cooled. The excess of water was added slowly at 25° C. for precipitation, the mixture was stirred for 2 hours and filtered. The filtered solid was recrystallized with isopropanol and ether, filtered and dried to give a desired compound of 2.17 g (yield: 78%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 12 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. customThe filtered solid was recrystallized with isopropanol and ether
  6. filtrationfiltered
  7. customdried

出典と根拠

ORDレコード
ord-3fec5f37eb44411584295af90c1ecc64
出典データセット
uspto-grants-2001_10
特許番号
US06306860B1

反応ノート

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