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

Sodium Bicarbonate → HCID 86724133, 화합물

HRID 1748804
노트
인쇄 미리보기

반응식

HRID 1748804 반응식
C([Li])CCC.[Cl-].[CH3:7][O:8][CH2:9][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Br:29][C:30]1[CH:35]=[CH:34][C:33]([CH:36]([C:40]2[C:41]([C:55]3[CH:60]=[CH:59][CH:58]=[CH:57][N:56]=3)=[N:42][N:43]([CH2:53][CH3:54])[C:44]=2[NH:45][C:46](=[O:52])[O:47][C:48]([CH3:51])([CH3:50])[CH3:49])[CH2:37][CH:38]=O)=[CH:32][CH:31]=1.C([O-])(O)=O.[Na+]>CCOC(C)=O.C1COCC1>[Br:29][C:30]1[CH:35]=[CH:34][C:33]([CH:36]([C:40]2[C:41]([C:55]3[CH:60]=[CH:59][CH:58]=[CH:57][N:56]=3)=[N:42][N:43]([CH2:53][CH3:54])[C:44]=2[NH:45][C:46](=[O:52])[O:47][C:48]([CH3:50])([CH3:51])[CH3:49])[CH2:37][CH:38]=[CH:7][O:8][CH3:9])=[CH:32][CH:31]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 516892Sodium BicarbonateHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 86724132HCID 86724132, 화합물HCID 178418339Butyllithium

생성물 1

HCID 86724133HCID 86724133, 화합물수율 82.1%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

n-Butyllithium (1.6 M solution in hexanes, 0.980 mL, 1.57 mmol) was added dropwise over about 10 min to a slurry of (methoxymethyl)triphenylphosphonium chloride (0.550 g, 1.60 mmol) and THF (3.00 mL) under N2 at about −78° C. After about 5 min, the reaction vessel was transferred to an ice water bath. After stirring for about 10 min at about 0° C., the dark red reaction mixture was cooled to about −78° C. A solution of tert-butyl (4-(1-(4-bromophenyl)-3-oxopropyl)-1-ethyl-3-(pyridin-2-yl)-1H-pyrazol-5-yl)carbamate (0.161 g, 0.168 mmol) and THF (1.50 mL) was added over about 5 min. After about 5 min, the reaction mixture was transferred to an ice bath. After about 1 h, saturated aqueous NaHCO3 (5 mL) and EtOAc (5 mL) were added respectively. The ice bath was removed. The layers were separated and the aqueous layer was extracted with EtOAc (5 mL). The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified on silica gel using a gradient of 10-50% EtOAc in heptane. The fractions containing product were combined and concentrated under reduced pressure to afford tert-butyl (4-(1-(4-bromophenyl)-4-methoxybut-3-en-1-yl)-1-ethyl-3-(pyridin-2-yl)-1H-pyrazol-5-yl)carbamate (0.0726 g, 0.138 mmol, 82%) as an ivory solid. Compound was about a 2.2:1 mixture of olefin isomers. LC-MS (Table 1, Method g) Rt=2.83 min; m/z 527 and 529 (M+H)+(Major) and Rt=2.87 min; m/z 527 and 529 (M+H)+ (Minor).

후처리

  1. customthe reaction vessel was transferred to an ice water bath
  2. customthe dark red reaction mixture
  3. temperaturewas cooled to about −78° C
  4. waitAfter about 5 min
  5. customthe reaction mixture was transferred to an ice bath
  6. waitAfter about 1 h
  7. customThe ice bath was removed
  8. customThe layers were separated
  9. extractionthe aqueous layer was extracted with EtOAc (5 mL)
  10. dry with materialThe combined organics were dried over Na2SO4
  11. filtrationfiltered
  12. concentrationconcentrated under reduced pressure
  13. customThe residue was purified on silica gel using a gradient of 10-50% EtOAc in heptane
  14. additionThe fractions containing product
  15. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c3ee71322fa04e56be88b50d14724574
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150592B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트