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Triethylamine → Benzyl N-(3-hydroxypropyl)carbamate

HRID 64931
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HRID 64931 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][OH:5].C(N(CC)CC)C.[CH2:13]([O:20][C:21](Cl)=[O:22])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(Cl)Cl>[CH2:13]([O:20][C:21]([NH:1][CH2:2][CH2:3][CH2:4][OH:5])=[O:22])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 90863-Amino-1-propanolHCID 10387Benzyl chloroformate

생성물 1

HCID 562256Benzyl N-(3-hydroxypropyl)carbamate수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 300 ml of methylene chloride was dissolved 50 g of 3-aminopropanol, and thereto were successively added dropwise 33 g of triethylamine and 57 g of benzyloxycarbonyl chloride at -10° C. to -5° C. At the same temperature, the resulting mixture was stirred for 1 hour and then further stirred at room temperature for 1 hour. Subsequently, the reaction mixture was washed successively with 100 ml of diluted hydrochloric acid and 100 ml of water, and thereafter dried over anhydrous magnesium sulfate, after which the solvent was removed by distillation under reduced pressure to obtain 60 g (yield 86%) of 3-(benzyloxycarbonylamino)propanol having a melting point of 55°-56° C.

후처리

  1. stirringfurther stirred at room temperature for 1 hour
  2. washSubsequently, the reaction mixture was washed successively with 100 ml of diluted hydrochloric acid and 100 ml of water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customafter which the solvent was removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-4704827fddd649e09efd5efb3119ee9d
출처 데이터셋
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04610983

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