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

HRID 2083763ノート

反応式

HRID 2083763 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ea2a40de98704208870f2e60807f27b1
出典データセット
uspto-grants-1978_04
特許番号
US04086350

反応ノート

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