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Pyridine → HCID 21444366, 화합물

HRID 328288
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HRID 328288 반응식
[Cl:1][C:2]1[N:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8]([N:12]3[CH:20]([OH:21])[C:19]4[C:14](=[CH:15][C:16]([C:22]([F:25])([F:24])[F:23])=[CH:17][CH:18]=4)[C:13]3=[O:26])=[N:9]2)=[CH:4][CH:3]=1.Cl.Cl[C:29]([N:31]1[CH2:36][CH2:35][N:34]([CH3:37])[CH2:33][CH2:32]1)=[O:30].C(N(CC)CC)C.N1C=CC=CC=1>C(Cl)Cl>[Cl:1][C:2]1[N:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8]([N:12]3[CH:20]([O:21][C:29]([N:31]4[CH2:36][CH2:35][N:34]([CH3:37])[CH2:33][CH2:32]4)=[O:30])[C:19]4[C:14](=[CH:15][C:16]([C:22]([F:24])([F:25])[F:23])=[CH:17][CH:18]=4)[C:13]3=[O:26])=[N:9]2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1049PyridineHCID 8471TriethylamineHCID 30169344-Methylpiperazine-1-carbonyl chloride monohydrochlorideHCID 227547182-(7-Chloro-1,8-naphthyridin-2-yl)-3-hydroxy-6-trifluoromethyl-1-isoindolinone

생성물 1

HCID 21444366HCID 21444366, 화합물수율 73.5%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

Following the procedure of Example 28, but starting from 2-(7-chloro-1,8-naphthyridin-2-yl)-3-hydroxy-6-trifluoromethyl-1-isoindolinone (4.8 g.), 1-chlorocarbonyl-4-methyl-piperazine hydrochloride (15.1 g.), triethylamine (14.2 cc., equivalent to 10.2 g.) and pyridine (66 cc.) in methylene chloride (250 cc.), a crude product (7.8 g.) is obtained, which is triturated with water (50 cc.). The solid obtained is filtered off and washed with water (30 cc.). After recrystallisation from isopropanol (240 cc.), 2-(7-chloro1,8-naphthyridin-2-yl)-3-(4-methyl-piperazinyl)carbonyloxy-6-trifluoromethyl-1-isoindolinone (4.7 g.) melting at 219° C is obtained.

후처리

  1. customa crude product (7.8 g.) is obtained
  2. customwhich is triturated with water (50 cc.)
  3. customThe solid obtained
  4. filtrationis filtered off
  5. washwashed with water (30 cc.)
  6. customAfter recrystallisation from isopropanol (240 cc.)

출처 및 근거

ORD 기록
ord-02ca71111948424b80d514902a0b2243
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04016274

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