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Ammonium Chloride → 2,6-Difluoro-9-(1-methylpiperidin-4-YL)-9H-thioxanthen-9-OL

HRID 2083770
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HRID 2083770 반응식
Cl[CH:2]1[CH2:7][CH2:6][N:5]([CH3:8])[CH2:4][CH2:3]1.[Mg].[F:10][C:11]1[CH:24]=[CH:23][C:22]2[S:21][C:20]3[C:15](=[CH:16][CH:17]=[C:18]([F:25])[CH:19]=3)[C:14](=[O:26])[C:13]=2[CH:12]=1.[Cl-].[NH4+]>O1CCCC1>[F:10][C:11]1[CH:24]=[CH:23][C:22]2[S:21][C:20]3[C:15](=[CH:16][CH:17]=[C:18]([F:25])[CH:19]=3)[C:14]([CH:2]3[CH2:7][CH2:6][N:5]([CH3:8])[CH2:4][CH2:3]3)([OH:26])[C:13]=2[CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 793424-chloro-N-methylpiperidineHCID 5462224MagnesiumHCID 203574842,6-Difluoro-9H-thioxanthen-9-one

생성물 1

HCID 203574792,6-Difluoro-9-(1-methylpiperidin-4-YL)-9H-thioxanthen-9-OL

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The Grignard reagent prepared from 2.7 g. (0.02 mol) of 4-chloro-N-methylpiperidine and 0.5 g. (0.02 mol) of magnesium turnings in tetrahydrofuran is treated with 2.5 g. (0.01 mol) of 2,6-difluorothioxanthone at a rate to maintain slow reflux. The mixture is refluxed for six hours, hydrolyzed with saturated ammonium chloride solution and extracted with ether to yield 2,6-difluoro-9-(1-methyl-4-piperidyl)-thioxanthene-9-ol, m.p. 207°-209° C.

후처리

  1. extractionextracted with ether

출처 및 근거

ORD 기록
ord-8ef1ec4c11af45f8b00f522d2b3e915a
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04086350

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