Acetate → 2-(2-Guanidinoethoxy)ethyl acetate

HRID 635553

반응식

HRID 635553 반응식
C(O)(=O)C[CH2:3][C:4]([OH:6])=[O:5].O[CH2:10][CH2:11][O:12][CH2:13][CH2:14][NH:15][C:16]([NH2:18])=[NH:17].C(OC(=O)C)(=O)C.C([O-])(=O)C>C(N(CC)CC)C>[C:4]([O:6][CH2:10][CH2:11][O:12][CH2:13][CH2:14][NH:15][C:16]([NH2:18])=[NH:17])(=[O:5])[CH3:3]

참가 물질

5

반응물 3

HCID 175AcetateHCID 7918Acetic AnhydrideHCID 178418465HCID 178418465, 화합물

생성물 1

HCID 1784182412-(2-Guanidinoethoxy)ethyl acetate수율 40%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

2.06 g (9.99 mmol) of 2-(2-hydroxyethoxy)ethylguanidine succinate, 8 ml of triethylamine, 0.122 mg (1.0 mmol) of 4-N,N-dimethylaminopyridine and 1.02 g (9.99 mmol) of acetic anhydride were placed in a 50 ml two neck flask and were stirred for 1 hour at room temperature. After the upper phase was removed by decantation, the obtained crude product was washed five times with 50 ml of diethylether. The product was purified by a silica gel column chromatography (eluent, chloroform/ethanol=2/1 containing 0.5% acetic acid) to obtain 1.00 g of the title compound (starch syrup-like, 4.0 mmol, 40.0% in yield) in the form of acetate. Results of the analysis of this compound are as follows.

후처리

  1. customAfter the upper phase was removed by decantation
  2. customthe obtained crude product
  3. washwas washed five times with 50 ml of diethylether
  4. customThe product was purified by a silica gel column chromatography (eluent, chloroform/ethanol=2/1 containing 0.5% acetic acid)

출처 및 근거

ORD 기록
ord-605fdc7c832c43279cd877d18b16064c
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06187955B1

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