Ammonium Chloride → 3-Fluoro-9-(1-methylpiperidin-4-yl)-9H-thioxanthen-9-ol

HRID 2083763노트

반응식

HRID 2083763 반응식
[Mg].Cl[CH:3]1[CH2:8][CH2:7][N:6]([CH3:9])[CH2:5][CH2:4]1.[F:10][C:11]1[CH:12]=[CH:13][C:14]2[C:15](=[O:25])[C:16]3[C:21]([S:22][C:23]=2[CH:24]=1)=[CH:20][CH:19]=[CH:18][CH:17]=3.[Cl-].[NH4+]>O1CCCC1>[F:10][C:11]1[CH:12]=[CH:13][C:14]2[C:15]([CH:3]3[CH2:8][CH2:7][N:6]([CH3:9])[CH2:5][CH2:4]3)([OH:25])[C:16]3[C:21]([S:22][C:23]=2[CH:24]=1)=[CH:20][CH:19]=[CH:18][CH:17]=3

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 793424-chloro-N-methylpiperidineHCID 5462224MagnesiumHCID 217304583-Fluoro-9H-thioxanthen-9-one

생성물 1

HCID 203575253-Fluoro-9-(1-methylpiperidin-4-yl)-9H-thioxanthen-9-ol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The Grignard reagent prepared from 0.62 g. of magnesium turnings and 3.5 g. of 4-chloro-N-methylpiperidine in tetrahydrofuran is treated with a solution of 3-fluoro-9-thioxanthone (3.0 g.) in 50 ml. of tetrahydrofuran. The mixture is refluxed for four hours, cooled, treated with saturated ammonium chloride solution and extracted with ether. The ether extract is washed with water, dried and concentrated to give 3-fluoro-9-(1-methyl-4-piperidyl)-thioxanthene-9-ol, m.p. 120°-130° C.

후처리

  1. temperatureThe mixture is refluxed for four hours
  2. temperaturecooled
  3. extractionextracted with ether
  4. extractionThe ether extract
  5. washis washed with water
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ea2a40de98704208870f2e60807f27b1
출처 데이터셋
uspto-grants-1978_04
특허 번호
US04086350

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