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

Ethyl Acetate → HCID 178481818, 화합물

HRID 271305
노트
인쇄 미리보기

반응식

HRID 271305 반응식
[C:1]([S:5]([NH2:7])=[O:6])([CH3:4])([CH3:3])[CH3:2].[Cl:8][C:9]1[CH2:10][CH:11]2[C:32](=O)[CH:14]([CH2:15][C:16]=1/[CH:17]=[CH:18]/[C:19]1[CH:23]=[C:22]([C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=3)[N:21]([CH3:31])[N:20]=1)[CH2:13][CH2:12]2.C(OCC)(=O)C>C1COCC1.[Cl-].[Na+].O.[O-]CC.[Ti+4].[O-]CC.[O-]CC.[O-]CC>[Cl:8][C:9]1[CH2:10][CH:11]2[CH2:12][CH2:13][CH:14](/[C:32]/2=[N:7]/[S:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[O:6])[CH2:15][C:16]=1/[CH:17]=[CH:18]/[C:19]1[CH:23]=[C:22]([C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)[N:21]([CH3:31])[N:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 8857Ethyl AcetateHCID 3382465Tert-ButanesulfinamideHCID 693100833-chloro-4-{(E)-2-[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-3-yl]vinyl}bicyclo[4.2.1]non-3-en-9-one

생성물 1

HCID 178481818HCID 178481818, 화합물수율 99.5%

시약·촉매·용매 3

HCID 76524Titanium tetraethoxide촉매
HCID 8028
Tetrahydrofuran
용매
HCID 57417360Sodium chloride; water용매

실험 절차

tert-Butylsulphinamide (3.0, 24 mmol) followed by titanium (IV) ethoxide (4.6 ml, 36 mmol) was added to a stirring solution of the product of Step 3 (4.56 g, 11 mmol) in dry THF (10 ml) and the resulting solution was heated to reflux for 18 hrs. The reaction was poured into a stirring solution of brine (200 ml) and then ethyl acetate (100 ml) was added and the mixture filtered through celite. The filtrate was partitioned and the aqueous layer was further extracted with ethyl acetate (2×50 ml). The combined organic extract was washed with brine, dried over MgSO4 and concentrated in vacuo, to afford N((9Z)-3-chloro-4-{(E)-2-[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-3-yl]vinyl}bicyclo[4.2.1]non-3-en-9-ylidene)-2-methylpropane-2-sulfinamide (5.19 g, 99%). m/z (ES+) 474 (MH)+. Compound taken directly onto next Step.

후처리

  1. temperaturethe resulting solution was heated
  2. temperatureto reflux for 18 hrs
  3. filtrationthe mixture filtered through celite
  4. customThe filtrate was partitioned
  5. extractionthe aqueous layer was further extracted with ethyl acetate (2×50 ml)
  6. extractionThe combined organic extract
  7. washwas washed with brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0c6df90edbba416b8afb216f35002d16
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07452899B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트