홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → HCID 15859997, 화합물

HRID 549783
노트
인쇄 미리보기

반응식

HRID 549783 반응식
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH2:13][C:14]([N:16]3[CH2:21][CH2:20][N:19]([C:22]4[C:27]5[CH:28]=[CH:29][S:30][C:26]=5[CH:25]=[CH:24][N:23]=4)[CH2:18][CH2:17]3)=O)=[CH:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[F:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH2:13][CH2:14][N:16]3[CH2:21][CH2:20][N:19]([C:22]4[C:27]5[CH:28]=[CH:29][S:30][C:26]=5[CH:25]=[CH:24][N:23]=4)[CH2:18][CH2:17]3)=[CH:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 25028976HCID 25028976, 화합물

생성물 1

HCID 15859997HCID 15859997, 화합물수율 64.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매
2회

실험 절차

107.7 kg (1 eq.) of intermediate 7-fluoro-4-[2-[4-(thieno[3,2-c]pyridin-4-yl)piperazin-1-yl]-2-oxoethyl]quinolin-2(1H)-one (I), followed by 3231 of THF, are introduced, in thirty minutes at 10° C., into a suspension of 22.2 kg (2.3 eq.) of lithium aluminium hydride in 580 l of tetrahydrofuran, in a reactor. The mixture is stirred for three hours at ambient temperature and then, after verification that the reaction is complete, the mixture is cooled and 21.5 l of water, 21.5 l of 4N sodium hydroxide and 180 l of water are added successively without the temperature exceeding 15° C. The mixture is stirred for one hour and the inorganic salts are filtered off. The mixture is concentrated to three volumes of THF and run into 1400 l of water. The mixture is filtered and a paste is re-formed in 1000 l of a water/THF mixture: 3/7. The product is dried under vacuum at 50° C. Compound (V) is obtained.

후처리

  1. temperaturethe mixture is cooled
  2. customexceeding 15° C
  3. stirringThe mixture is stirred for one hour
  4. filtrationthe inorganic salts are filtered off
  5. concentrationThe mixture is concentrated to three volumes of THF
  6. filtrationThe mixture is filtered
  7. customa paste is re-formed in 1000 l of a water/THF mixture
  8. customThe product is dried under vacuum at 50° C

출처 및 근거

ORD 기록
ord-8a4f2e7d28484de284e89c28b49d7f29
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07943769B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트