Acetic Acid → HCID 178517892、化合物

HRID 70094

反応式

HRID 70094 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(O)(=O)C.CS[C:20]1[N:21]=[C:22]([OH:29])[C:23]2[S:28][CH2:27][CH2:26][C:24]=2[N:25]=1>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:20]3[N:21]=[C:22]([OH:29])[C:23]4[S:28][CH2:27][CH2:26][C:24]=4[N:25]=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 178503521HCID 178503521、化合物

生成物 1

HCID 178517892HCID 178517892、化合物収率 92.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
180 °C

実験手順

20.45 g 1-(4-chloro-phenyl)-piperazine are placed in 5.95 ml (104 mmol) glacial acetic acid and heated to 180° C. 8.01 g 2-methylsulphanyl-6,7-dihydro-thieno[3,2-d]pyrimidin-4-ol are added, the non-stirrable reaction mixture is heated for 2.5 hours to 180° C. After cooling, water is added, the precipitate is suction filtered and dried in the air. The substance is treated with ethanol under ultrasound, suction filtered and dried. 12.95 g of the product are obtained as a powder.

後処理

  1. temperaturethe non-stirrable reaction mixture is heated for 2.5 hours to 180° C
  2. temperatureAfter cooling
  3. filtrationfiltered
  4. customdried in the air
  5. additionThe substance is treated with ethanol under ultrasound, suction
  6. filtrationfiltered
  7. customdried

出典と根拠

ORDレコード
ord-115cf9f5eb3a4b0b9a4d930d5c814dda
出典データセット
uspto-grants-2014_09
特許番号
US08822474B2

関連ノート

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