Ethyl Bromide → HCID 20357511, 화합물

HRID 2083756노트

반응식

HRID 2083756 반응식
[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

참가 물질

7

반응물 5

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

생성물 1

HCID 20357511HCID 20357511, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-665fd8c5b1cd425494e5416da5445bd1
출처 데이터셋
uspto-grants-1978_04
특허 번호
US04086350

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