Acetic Acid → HCID 178517892、化合物

HRID 1805993ノート

反応式

HRID 1805993 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[C:14]([OH:17])(=O)[CH3:15].Cl[C:19]1[N:20]=C(NC2C=C(C=CC=2)C(O)=O)C2[S:27][CH2:26][CH2:25][C:23]=2[N:24]=1>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:19]3[N:20]=[C:14]([OH:17])[C:15]4[S:27][CH2:26][CH2:25][C:23]=4[N:24]=3)[CH2:10][CH2:9]2)=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 974781-(4-Chlorophenyl)piperazineHCID 576001073-(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-ylamino)benzoic acid

生成物 1

HCID 178517892HCID 178517892、化合物収率 96.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
180 °C

実験手順

1.9 g (9.66 mmol) of 1-(4-chlorophenyl)piperazine is placed in 0.55 mL (9.62 mmol) of glacial acetic acid and heated to 180° C. in the heating block. 0.800 g (3.73 mmol) of 2-ethylsulfanyl-6,7-dihydrothieno[3,2-d]pyrimidin-4-ol (I) is added, then the mixture is left to stand for 1.5 hours at 180° C. and 16 hours at ambient temperature. Then the reaction mixture is combined with water and treated in the ultrasound bath. The precipitate is suction filtered, washed, and dried. 1.25 g of product II is obtained and used further in the crude state.

後処理

  1. waitthe mixture is left
  2. additiontreated in the ultrasound bath
  3. filtrationfiltered
  4. washwashed
  5. customdried

出典と根拠

ORDレコード
ord-f0845963e50b4252917224014cbdd133
出典データセット
uspto-grants-2013_01
特許番号
US08354531B2

反応ノート

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