Water → HCID 68574900、化合物

HRID 656462ノート

反応式

HRID 656462 の反応式
Cl.[NH2:2][CH2:3][C:4]1([CH2:12][C:13]([OH:15])=O)[CH2:9][CH2:8][CH2:7][CH:6]([CH2:10][NH2:11])[NH:5]1.C(N(C(C)C)C(C)C)C.CCCP(=O)=O.O>C(OCC)(=O)C>[NH2:11][CH2:10][CH:6]1[CH2:7][CH2:8][CH2:9][C:4]2([CH2:3][NH:2][C:13](=[O:15])[CH2:12]2)[NH:5]1

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 16167369Propylphosphoric anhydrideHCID 68575364HCID 68575364、化合物

生成物 1

HCID 68574900HCID 68574900、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A suspension of 5.590 mmol of (2,6-bis-aminomethylpiperidin-2-yl)acetic acid hydrochloride and 22.340 mmol of N-ethyldiisopropylamine in 20 ml of ethyl acetate is admixed dropwise at 0° C. with a solution of 11.170 mmol of propylphosphonic anhydride (T3P®) (50% w/w in ethyl acetate). The reaction mixture is subsequently stirred at room temperature for 20 h. It is admixed with water (20 ml) the organic phase is separated off and the aqueous phase is extracted with ethyl acetate (3×). The combined organic phases are dried over sodium sulphate and evaporated. From the residue the title compound is obtained by means of flash chromatography (SiO2 60 F) and identified on the basis of the Rf value.

後処理

  1. customis separated off
  2. extractionthe aqueous phase is extracted with ethyl acetate (3×)
  3. dry with materialThe combined organic phases are dried over sodium sulphate
  4. customevaporated

出典と根拠

ORDレコード
ord-6cc821caaf0543ffbb6bc16e593660f3
出典データセット
uspto-grants-2011_12
特許番号
US08071773B2

反応ノート

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