Water → HCID 68574900, 화합물

HRID 656462노트

반응식

HRID 656462 반응식
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

참가 물질

6

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 16167369Propylphosphoric anhydrideHCID 68575364HCID 68575364, 화합물

생성물 1

HCID 68574900HCID 68574900, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6cc821caaf0543ffbb6bc16e593660f3
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071773B2

반응 노트

불러오는 중…