Ethyl Bromide → HCID 20357511、化合物

HRID 2083756ノート

反応式

HRID 2083756 の反応式
[Mg].Cl[CH:3]1[CH2:8][CH2:7][N:6]([CH3:9])[CH2:5][CH2:4]1.C(Br)C.[Br:13][C:14]1[CH:27]=[CH:26][C:25]2[S:24][C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17](=[O:28])[C:16]=2[CH:15]=1.[Cl-].[NH4+]>O1CCCC1>[Br:13][C:14]1[CH:27]=[CH:26][C:25]2[S:24][C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17]([CH:3]3[CH2:8][CH2:7][N:6]([CH3:9])[CH2:5][CH2:4]3)([OH:28])[C:16]=2[CH:15]=1

参加物

7

反応物 5

HCID 6332Ethyl BromideHCID 25517Ammonium ChlorideHCID 793424-chloro-N-methylpiperidineHCID 3181012-Bromo-10-thiaxanthenoneHCID 5462224Magnesium

生成物 1

HCID 20357511HCID 20357511、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 1.2 l g. (0.05 mol) of magnesium turnings covered by tetrahydrofuran in an Argon atmosphere is added about 0.5 g. of 4-chloro-N-methylpiperidine (from 8.5 g., 0.025 mol of the hydrochloride salt) and a small amount of ethyl bromide. The mixture is heated until the reaction is initiated, the remainder of the chloro compound in about 20 ml. of tetrahydrofuran is added and the mixture is refluxed for four hours. 2-Bromothioxanthone (7.3 g., 0.025 mol) is added and the mixture is refluxed for five hours, and then stirred at room temperature 3 days. The reaction mixture is poured into aqueous ammonium chloride and filtered to give 2-bromo-9(1-methyl-4-piperidyl)thioxanthene-9-ol, m.p. 225.5°-226° C.

後処理

  1. additionis added about 0.5 g
  2. temperatureThe mixture is heated until the reaction
  3. temperaturethe mixture is refluxed for four hours
  4. temperaturethe mixture is refluxed for five hours
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-665fd8c5b1cd425494e5416da5445bd1
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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