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

Potassium Carbonate → 3-{4-[2-(4-Nitro-phenyl)-ethyl]-piperazin-1-YL}-1,2-benzisothiazole

HRID 2211857
노트
인쇄 미리보기

반응식

HRID 2211857 반응식
C(=O)([O-])[O-].[K+].[K+].Cl.[N:8]1([C:14]2[C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=3[S:16][N:15]=2)[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.S(C1C=CC(C)=CC=1)(O[CH2:27][CH2:28][C:29]1[CH:34]=[CH:33][C:32]([N+:35]([O-:37])=[O:36])=[CH:31][CH:30]=1)(=O)=O>CC(C)=O.C1OCCOCCOCCOCCOCCOC1>[N+:35]([C:32]1[CH:33]=[CH:34][C:29]([CH2:28][CH2:27][N:11]2[CH2:12][CH2:13][N:8]([C:14]3[C:18]4[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=4[S:16][N:15]=3)[CH2:9][CH2:10]2)=[CH:30][CH:31]=1)([O-:37])=[O:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 2447744-Nitrophenethyl tosylateHCID 115217113-(1-Piperazinyl)-1,2-benzisothiazole monohydrochloride

생성물 1

HCID 219632673-{4-[2-(4-Nitro-phenyl)-ethyl]-piperazin-1-YL}-1,2-benzisothiazole수율 86.7%

시약·촉매·용매 2

HCID 2855718-Crown-6촉매
HCID 180
Acetone
용매

실험 절차

Excess dried, −325 mesh potassium carbonate (20 g) was diluted in 500 mL acetone and 3-piperazin-1-yl-benzoisothiazole hydrochloride (13.05 g, 51.2 mmol) was added. The mixture was stirred for 15 min before 4-nitrophenethyl tosylate (14.93 g, 46.5 mmol) and catalytic 18-crown-6 (0.5 g, 1.9 mmol) was added. The mixture was stirred at reflux for 42 h. After cooling, the salts were filtered off and washed with acetone and the filtrate was concentrated. The residue was taken up in methylene chloride and washed with water. The organic layer was dried over sodium sulfate, and concentrated. The residue was triturated with ethyl acetate and the collected solid was washed with ethyl ether and dried in vacuo to afford 14.86 g of a bright yellow solid. Yield 84%; mp 99° C.; MS (APCI): 369 [M+H]+.

후처리

  1. additionwas added
  2. temperatureat reflux for 42 h
  3. temperatureAfter cooling
  4. filtrationthe salts were filtered off
  5. washwashed with acetone
  6. concentrationthe filtrate was concentrated
  7. washwashed with water
  8. dry with materialThe organic layer was dried over sodium sulfate
  9. concentrationconcentrated
  10. customThe residue was triturated with ethyl acetate
  11. washthe collected solid was washed with ethyl ether
  12. customdried in vacuo

출처 및 근거

ORD 기록
ord-372a987f120e4e6ba551a73042d498a9
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07101886B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트