Sodium → HCID 178523047, 화합물

HRID 1949151노트

반응식

HRID 1949151 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178523047HCID 178523047, 화합물수율 90%

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-49a84d860be34ad88bab140df2c071e9
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399673B2

반응 노트

불러오는 중…