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Triethylamine → Benzyl N-(3-hydroxypropyl)carbamate

HRID 64931
ノート
印刷プレビュー

反応式

HRID 64931 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 562256Benzyl N-(3-hydroxypropyl)carbamate収率 86%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4704827fddd649e09efd5efb3119ee9d
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04610983

反応ノート

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