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

Pyridine → 2-Chloro-4-fluoro-N-[3-(1-methyl-piperidin-4-ylsulfanyl)-phenyl]-benzamide hydrogen chloride salt

HRID 1822057
노트
인쇄 미리보기

반응식

HRID 1822057 반응식
N1C=CC=CC=1.[CH3:7][N:8]1[CH2:13][CH2:12][CH:11]([S:14][C:15]2[CH:16]=[C:17]([NH2:21])[CH:18]=[CH:19][CH:20]=2)[CH2:10][CH2:9]1.[Cl:22][C:23]1[CH:31]=[C:30]([F:32])[CH:29]=[CH:28][C:24]=1[C:25](Cl)=[O:26]>ClCCl>[ClH:22].[Cl:22][C:23]1[CH:31]=[C:30]([F:32])[CH:29]=[CH:28][C:24]=1[C:25]([NH:21][C:17]1[CH:18]=[CH:19][CH:20]=[C:15]([S:14][CH:11]2[CH2:10][CH2:9][N:8]([CH3:7])[CH2:13][CH2:12]2)[CH:16]=1)=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 27365462-Chloro-4-fluorobenzoyl chlorideHCID 450977713-[(1-Methyl-4-piperidinyl)sulfanyl]aniline

생성물 1

HCID 690724312-Chloro-4-fluoro-N-[3-(1-methyl-piperidin-4-ylsulfanyl)-phenyl]-benzamide hydrogen chloride salt

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Combine pyridine (0.110 mL, 1.36 mmol), 3-(1-methyl-piperidin-4-ylsulfanyl)-phenylamine (preparation 76,151 mg, 0.679 mmol) in dichloromethane (6.5 mL) at 0° C. Stir and add 2-chloro-4-fluorobenzoyl chloride (0.105 mL, 0.815 mmol). Allow to warm to ambient temperature and stir. After 2 hr., dilute with dichloromethane (10 mL) and wash with sodium hydroxide (1N, 3×10 mL). Combine the organic layers, dry over sodium sulfate and concentrate under reduced pressure. Purification by flash chromatography, eluting with dichloromethane/ammonia (2.0 N in methanol) [20/1] to give the title compound as free base (184 mg, 72%). Dissolve the residue in diethyl ether and treat with ethereal hydrogen chloride (1.0 M). Triturate the resulting gum with ether to give the title compound as the hydrogen chloride salt. 1H NMR (free base, CDCl3): 8.37 (bs, 1H), 7.65 (s, 1H), 7.58 (t, J=6.8 Hz, 1H), 7.42 (d, J=7.7 Hz, 1H), 7.21 (t, J=7.8 Hz, 1H), 7.14-7.06 (m, 2H), 6.99-6.93 (m, 1H), 3.05 (bs, 1H), 2.71 (bd, J=11.5 Hz, 2H), 2.19 (s, 3H), 2.03-1.90 (m, 4H), 1.67-1.56 (m, 2H). 13C NMR (free base, CDCl3): 164.9, 162.2 (d, JC-F=167.7 Hz), 137.9, 135.8, 132.0, 131.7 (d, JC-F=8.6 Hz), 131.4, 129.3, 128.0, 123.0, 118.6, 117.5 (d, JC-F=25.0 Hz), 114.5 (d, JC-F=21.3 Hz), 54.9, 46.0, 43.6, 32.4.

후처리

  1. customat 0° C
  2. stirringstir
  3. washwash with sodium hydroxide (1N, 3×10 mL)
  4. dry with materialCombine the organic layers, dry over sodium sulfate
  5. concentrationconcentrate under reduced pressure
  6. customPurification by flash chromatography
  7. washeluting with dichloromethane/ammonia (2.0 N in methanol) [20/1]

출처 및 근거

ORD 기록
ord-70c28b2da06043b3adbbe5b52b66f96f
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07608629B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트