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Water → HCID 12466834, 화합물

HRID 1679433
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HRID 1679433 반응식
[OH:1][CH2:2][CH2:3][N:4]1[CH2:8][CH2:7][O:6][CH:5]1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[Mg].[CH3:16][O:17][C:18]1[CH:19]=[C:20]([CH:23]=[CH:24][CH:25]=1)[CH2:21]Cl.O>CCOCC>[OH:1][CH2:2][CH2:3][N:4]([CH:5]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH2:21][C:20]1[CH:23]=[CH:24][CH:25]=[C:18]([O:17][CH3:16])[CH:19]=1)[CH2:8][CH2:7][OH:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 699943-Methoxybenzyl chlorideHCID 5462224MagnesiumHCID 126486632-(2-Phenyl-1,3-oxazolidin-3-yl)ethan-1-ol

생성물 1

HCID 12466834HCID 12466834, 화합물수율 70.7%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 3-(2-hydroxyethyl)-2-phenyloxazolidine (11.0 g) in anhydrous ether (30 ml) is added dropwise with stirring to Grignard reagent which is prepared from magnesium turnings (3.3 g) and m-methoxybenzyl chloride (20.7 g) in anhydrous ether (150 ml), and the mixture is refluxed for 3 hours. After the reaction, the reaction mixture is decomposed by adding water thereto. The ether layer is separated and extracted with 10% hydrochloric acid (100 ml). The hydrochloric acid layer is made alkaline with ammonia and extracted with ether. The ether layer is dried over anhydrous sodium sulfate, and the solvent is distilled off to give crude dl-N,N-bis(2-hydroxyethyl)-2-(3-methoxyphenyl)-1-phenylethylamine (12.7 g) as an oily substance. When this substance is recrystallized from ethanol, it shows a melting point of 67°-69° C.

후처리

  1. temperaturethe mixture is refluxed for 3 hours
  2. customAfter the reaction
  3. customThe ether layer is separated
  4. extractionextracted with 10% hydrochloric acid (100 ml)
  5. extractionextracted with ether
  6. dry with materialThe ether layer is dried over anhydrous sodium sulfate
  7. distillationthe solvent is distilled off

출처 및 근거

ORD 기록
ord-c6203a5dd0a94b86bea703474d3cbca6
출처 데이터셋
uspto-grants-1978_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04080453

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