Sodium → HCID 178523047、化合物

HRID 1949151ノート

反応式

HRID 1949151 の反応式
[Na].COC(=O)CC[S:7][C:8]1[C:17]([C:18](=[O:26])[NH:19][CH2:20][C:21]2[S:22][CH:23]=[CH:24][CH:25]=2)=[CH:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9]=1>CO>[SH:7][C:8]1[C:17]([C:18]([NH:19][CH2:20][C:21]2[S:22][CH:23]=[CH:24][CH:25]=2)=[O:26])=[CH:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9]=1

参加物

4

反応物 2

HCID 5360545SodiumHCID 594862173-[[3-[Oxo-(2-thienylmethylamino)methyl]-2-quinolyl]thio]propanoic acid methyl ester

生成物 1

HCID 178523047HCID 178523047、化合物収率 90%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
70 °C

実験手順

600 mg (26.1 mmol) sodium were added slowly to MeOH (500 ml). Then a solution of 1.16 g (3.0 mmol) 3-[[3-[oxo-(2-thienylmethylamino)methyl]-2-quinolyl]-thio]propanoic acid methyl ester (Example 2) in MeOH (60 ml) was added at RT. Then the reaction solution was heated for 1 h at 70° C. After cooling to RT the mixture was concentrated to small volume under vacuum. The residue was taken up with water and the solution was washed with EE. Then it was acidified with concentrated hydrochloric acid to pH 3. The deposit formed was filtered off and dried. 805 mg (2.7 mmol, 90%) 2-mercapto-N-(thiophen-2-ylmethyl)quinoline-3-carboxamide were obtained.

後処理

  1. temperatureAfter cooling to RT the mixture
  2. concentrationwas concentrated to small volume under vacuum
  3. washthe solution was washed with EE
  4. customThe deposit formed
  5. filtrationwas filtered off
  6. customdried

出典と根拠

ORDレコード
ord-49a84d860be34ad88bab140df2c071e9
出典データセット
uspto-grants-2013_03
特許番号
US08399673B2

反応ノート

読み込み中…