Acetate → 2-(2-Guanidinoethoxy)ethyl acetate

HRID 635553

反応式

HRID 635553 の反応式
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]

参加物

5

反応物 3

HCID 175AcetateHCID 7918Acetic AnhydrideHCID 178418465HCID 178418465、化合物

生成物 1

HCID 1784182412-(2-Guanidinoethoxy)ethyl acetate収率 40%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-605fdc7c832c43279cd877d18b16064c
出典データセット
uspto-grants-2001_02
特許番号
US06187955B1

関連ノート

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