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

Dimethyl Sulfoxide → HCID 22257971, 화합물

HRID 1611042
노트
인쇄 미리보기

반응식

HRID 1611042 반응식
CS(C)=O.[C:5](Cl)(=[O:9])[C:6](Cl)=O.OC[CH2:13][CH2:14][S:15][C:16]1[C:24]2[C:23](=[O:25])[N:22]([CH3:26])[C:21](=[O:27])[N:20]([CH2:28][CH:29]([CH3:31])[CH3:30])[C:19]=2[S:18][C:17]=1[CH2:32][C:33]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:36]=[CH:35][CH:34]=1.C(N(CC)CC)C>ClCCl.CCOCC>[OH:9][CH:5]([CH3:6])[CH2:13][CH2:14][S:15][C:16]1[C:24]2[C:23](=[O:25])[N:22]([CH3:26])[C:21](=[O:27])[N:20]([CH2:28][CH:29]([CH3:31])[CH3:30])[C:19]=2[S:18][C:17]=1[CH2:32][C:33]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:36]=[CH:35][CH:34]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 52825395-(3-Hydroxypropylsulfanyl)-3-methyl-1-(2-methylpropyl)-6-(naphthalen-1-ylmethyl)thieno[2,3-d]pyrimidine-2,4-dione

생성물 1

HCID 22257971HCID 22257971, 화합물

시약·촉매·용매 2

HCID 3283
Diethyl Ether
용매
HCID 6344Dichloromethane용매3회

실험 절차

A solution of dimethylsulfoxide (0.113 ml) in anhydrous dichloromethane (1 ml) was added to a solution of oxalyl chloride (0.093 ml) in anhydrous dichloromethane (5 ml) at −78° C. under nitrogen. After 5 minutes, a solution of 5-[(3-hydroxypropyl)thio]-3-methyl-1-(2-methylpropyl)-6-(1-naphthalenylmethyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (0.25 g) in anhydrous dichloromethane (4 ml) was added dropwise. After 10 minutes, triethylamine (0.372 ml) was added and the mixture was warmed to room temperature. Ether (30 ml) was added and the mixture was washed with 2M hydrochloric acid (10 ml) then with saturated sodium hydrogen carbonate solution (10 ml), then dried over anhydrous magnesium sulfate, filtered and evaporated. The residue was dissolved in anhydrous tetrahydrofuran (10 ml), cooled to −78° C. under nitrogen and treated with methyl magnesium chloride (3.0M is solution in tetrahydrofuran, 0.265 ml). The mixture was warmed to room temperature, then added to saturated sodium hydrogen carbonate solution (30 ml) and then extracted with ethyl acetate (2×30 ml). The organic extracts were dried over anhydrous magnesium sulfate, filtered through a small silica pad and evaporated. The residue was purified by preparative normal-phase HPLC with ethyl acetate/isohexane gradient elution followed by recrystallisation from ethyl acetate/isohexane to give the title compound (58 mg).

후처리

  1. waitAfter 10 minutes
  2. washthe mixture was washed with 2M hydrochloric acid (10 ml)
  3. dry with materialwith saturated sodium hydrogen carbonate solution (10 ml), then dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. dissolutionThe residue was dissolved in anhydrous tetrahydrofuran (10 ml)
  7. temperaturecooled to −78° C. under nitrogen
  8. additiontreated with methyl magnesium chloride (3.0M is solution in tetrahydrofuran, 0.265 ml)
  9. temperatureThe mixture was warmed to room temperature
  10. additionadded to saturated sodium hydrogen carbonate solution (30 ml)
  11. extractionextracted with ethyl acetate (2×30 ml)
  12. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  13. filtrationfiltered through a small silica pad
  14. customevaporated
  15. customThe residue was purified by preparative normal-phase HPLC with ethyl acetate/isohexane gradient elution
  16. customfollowed by recrystallisation from ethyl acetate/isohexane

출처 및 근거

ORD 기록
ord-3f968437ed5946ccad79e14aad9cf183
출처 데이터셋
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06984644B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트