4-Methylpiperazine-1-carbothioamide → 3-[2-(4-Methylpiperazin-1-yl)-1,3-thiazol-4-yl]benzoic acid

HRID 606602ノート

反応式

HRID 606602 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8](=[S:10])[NH2:9])[CH2:4][CH2:3]1.Br[CH2:12][C:13]([C:15]1[CH:16]=[C:17]([CH:21]=[CH:22][CH:23]=1)[C:18]([OH:20])=[O:19])=O>C1COCC1>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[S:10][CH:12]=[C:13]([C:15]3[CH:16]=[C:17]([CH:21]=[CH:22][CH:23]=3)[C:18]([OH:20])=[O:19])[N:9]=2)[CH2:4][CH2:3]1

参加物

4

反応物 2

HCID 21130864-Methylpiperazine-1-carbothioamideHCID 27568353-(Bromoacetyl)benzoic acid

生成物 1

HCID 582569803-[2-(4-Methylpiperazin-1-yl)-1,3-thiazol-4-yl]benzoic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4-Methyl-piperazine-1-carbothioic acid amide (2.47 mmol) and 3-(2-Bromo-acetyl)-benzoic acid (2.47 mmol) were mixed in THF (12 mL). After stirring at room temperature for 5 minutes the mixture was heated to 80° C. for 2 hours. The mixture was then cooled to room temperature and filtered. The solid was washed with a small amount of diethylether and dried. m/z=304.1 in MS ES+, which was characterized by hplc and MS and used in the next step without any further purification.

後処理

  1. temperaturewas heated to 80° C. for 2 hours
  2. temperatureThe mixture was then cooled to room temperature
  3. filtrationfiltered
  4. washThe solid was washed with a small amount of diethylether
  5. customdried
  6. customused in the next step without any further purification

出典と根拠

ORDレコード
ord-fc3c537173884a8282b26ffd820a6db2
出典データセット
uspto-grants-2011_03
特許番号
US07915300B2

反応ノート

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