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

Sodium Carbonate → HCID 44517832, 화합물

HRID 1951122
노트
인쇄 미리보기

반응식

HRID 1951122 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:12][N:11]([C:13]([CH:15]3[CH2:20][CH2:19][N:18]([CH2:21][CH2:22][CH2:23]SC)[CH2:17][CH2:16]3)=[O:14])[CH2:10][CH:9]2[N:26]([CH3:41])[C:27](=[O:40])[C:28]2[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[C:30]([C:36]([F:39])([F:38])[F:37])[CH:29]=2)=[CH:4][CH:3]=1.Cl[C:43]1C=CC=C(C(OO)=O)C=1.[S:53](=[O:57])(=O)(O)[O-:54].[Na+].C(=O)([O-])[O-].[Na+].[Na+]>ClCCl.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:12][N:11]([C:13]([CH:15]3[CH2:16][CH2:17][N:18]([CH2:21][CH2:22][CH2:23][S:53]([CH3:43])(=[O:57])=[O:54])[CH2:19][CH2:20]3)=[O:14])[CH2:10][CH:9]2[N:26]([CH3:41])[C:27](=[O:40])[C:28]2[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[C:30]([C:36]([F:37])([F:39])[F:38])[CH:29]=2)=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10340Sodium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 516919Sodium BisulfateHCID 67025603HCID 67025603, 화합물

생성물 1

HCID 44517832HCID 44517832, 화합물수율 83%

시약·촉매·용매 2

HCID 962Water
용매
HCID 6344Dichloromethane용매

실험 절차

To a solution of N-{(3RS,4SR)-4-(4-chloro-phenyl)-1-[1-(3-methylsulfanyl-propyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-4-methoxy-N-methyl-3-trifluoromethyl-benzamide (80 mg, 0.13 mmol) in dichloromethane (2 mL) was added under an atmosphere of nitrogen m-chloroperbenzoic acid (47 mg, 0.27 mmol) and stirred for 3 d at ambient temperature. Further addition of m-chloroperbenzoic acid (47 mg, 0.27 mmol) was followed by stirring for 3 h at ambient temperature. After the addition of an aqueous saturated solution of sodium bisulfate (10 mL) and water (10 mL) it was stirred for 1 h at ambient temperature. The reaction mixture was basified by addition of an aqueous solution of sodium carbonate (1 M). The aqueous layer was extracted with dichloromethane (20 mL) and the organic layers were washed with water (15 mL) and dried over sodium sulfate. Purification by chromatography (SiO2, heptane:(ethyl acetate:triethylamine=95:5):methanol=20:80:0 to 0:85:15) afforded the title compound (70 mg, 83%) as a light brown oil. MS m/e: 644.2 [M]+.

후처리

  1. stirringby stirring for 3 h at ambient temperature
  2. stirringwas stirred for 1 h at ambient temperature
  3. extractionThe aqueous layer was extracted with dichloromethane (20 mL)
  4. washthe organic layers were washed with water (15 mL)
  5. dry with materialdried over sodium sulfate
  6. customPurification by chromatography (SiO2, heptane:(ethyl acetate:triethylamine=95:5):methanol=20:80:0 to 0:85:15)

출처 및 근거

ORD 기록
ord-5ef31a8228e74b8485b2fbde7fa65ca5
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404679B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트