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Benzyl chloroformate → HCID 178465414、化合物

HRID 1936551
ノート
印刷プレビュー

反応式

HRID 1936551 の反応式
[NH2:1][CH:2]([PH:4](=[O:6])[OH:5])[CH3:3].Cl[C:8]([O:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:9]>O1CCOCC1.O>[C:12]1([CH2:11][O:10][C:8]([NH:1][CH:2]([PH:4](=[O:5])[OH:6])[CH3:3])=[O:9])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 10387Benzyl chloroformateHCID 3018298Aminoethylphosphinic acid

生成物 1

HCID 178465414HCID 178465414、化合物収率 73.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
20 °C

実験手順

To a solution of 1.7 g (15.6 mmol) of 1-aminoethyl phosphinic acid in 35 ml of a mixture of dioxane and water, in the presence of an equivalent of soda (624 mg), there is added, 0° C., dropwise and simultaneously, a solution of 3.1 g (18.3 mmol) of benzyl chloroformate in 9 ml of dioxane and, so as to maintain the pH of the reaction about 9, a solution of 1 g of soda in 8.7 ml of water. At the end of the addition, the mixture is maintained at a temperature about 20° C. for 2 hours. The aqueous phase is then washed 3 times with 20 ml of diethyl ether. The aqueous phase is acidified, at 0° C., with brisk agitation, with 11 ml of a 6N hydrochloric acid solution. An abundant white precipitate forms, which is filtered, washed with water and dried. There is recovered 2.8 g of product (yield=73.9%).

後処理

  1. customthe pH of the reaction about 9
  2. additionAt the end of the addition
  3. washThe aqueous phase is then washed 3 times with 20 ml of diethyl ether
  4. customis acidified, at 0° C., with brisk agitation, with 11 ml of a 6N hydrochloric acid solution
  5. filtrationAn abundant white precipitate forms, which is filtered
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-ddedc22613d148eda6d821f8dac8e4b8
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06391866B1

反応ノート

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