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

Hydrochloric Acid → HCID 21258162, 화합물

HRID 635207
노트
인쇄 미리보기

반응식

HRID 635207 반응식
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH3:20])[C:13](=[O:21])[N:12]([CH2:22][CH2:23][C:24]([O:26]C)=[O:25])[C:11]=2[N:10]=[C:9]1[C:28]([CH3:31])([CH3:30])[CH3:29])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O1CCCC1.[Li+].[OH-].Cl>O>[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH3:20])[C:13](=[O:21])[N:12]([CH2:22][CH2:23][C:24]([OH:26])=[O:25])[C:11]=2[N:10]=[C:9]1[C:28]([CH3:29])([CH3:31])[CH3:30])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 21258170HCID 21258170, 화합물

생성물 1

HCID 21258162HCID 21258162, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
5 °C

실험 절차

4.6 g (10.8 mmol) of 7-benzyl-8-(tert.-butyl)-3-(2-methoxycarbonylethyl)-1-n-propyl-xanthine are dissolved 50 ml of tetrahydrofuran and 120 ml of water and 3.24 g of LiOH×H2O are added successively with stirring. After about 16 hours' stirring at ambient temperature, the mixture is cooled to about 5° C. and adjusted to pH 5 with 2N HCl (aq.). The organic solvent is largely distilled off in vacuo and the aqueous phase remaining is extracted twice with 150 ml of dichloromethane. The organic phase is dried over MgSO4 and the solvent is distilled off in vacuo. The crude product remaining is purified by chromatography on silica gel (dichloromethane:methanol 90:10). Yield: 3.1 g (88%), amorphous solid.

후처리

  1. additionare added successively
  2. stirringAfter about 16 hours' stirring at ambient temperature
  3. distillationThe organic solvent is largely distilled off in vacuo
  4. extractionthe aqueous phase remaining is extracted twice with 150 ml of dichloromethane
  5. dry with materialThe organic phase is dried over MgSO4
  6. distillationthe solvent is distilled off in vacuo
  7. customThe crude product remaining is purified by chromatography on silica gel (dichloromethane:methanol 90:10)

출처 및 근거

ORD 기록
ord-220995ad001d491aaf6c9c599d67e47d
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06187780B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트