Triethylamine → 2,2-Dimethyl-5-oxo-3-(2-oxo-1-pyrrolidineacetyl)-1-imidazolidineacetamide

HRID 256364ノート

反応式

HRID 256364 の反応式
[O:1]=[C:2]1[CH2:6][CH2:5][CH2:4][N:3]1[CH2:7][C:8]([OH:10])=O.C(N(CC)CC)C.ClC(OCCCC)=O.[CH3:26][C:27]1([CH3:37])[NH:31][CH2:30][C:29](=[O:32])[N:28]1[CH2:33][C:34]([NH2:36])=[O:35]>CN(C)C=O>[CH3:26][C:27]1([CH3:37])[N:31]([C:8](=[O:10])[CH2:7][N:3]2[CH2:4][CH2:5][CH2:6][C:2]2=[O:1])[CH2:30][C:29](=[O:32])[N:28]1[CH2:33][C:34]([NH2:36])=[O:35]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 61140Butyl chloroformateHCID 31466872-(2-Oxopyrrolidin-1-yl)acetic acidHCID 201554662,2-Dimethyl-5-oxo-1-imidazolidineacetamide

生成物 1

HCID 201637092,2-Dimethyl-5-oxo-3-(2-oxo-1-pyrrolidineacetyl)-1-imidazolidineacetamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

An ice cold solution of 2-oxo-1-pyrrolidineacetic acid (1.45 g) and triethylamine (1.45 ml) in dimethylformamide (7 ml) was treated dropwise while stirring with butyl chloroformate (1.3 ml). After stirring at 0° C. for 45 minutes, 2,2-dimethyl-5-oxo-1-imidazolidineacetamide (1.75 g) was added at once and stirring was prolonged at room temperature overnight. After evaporation under reduced pressure, the residue was chromatographed on a silica gel column, eluting with dichloromethane/methanol 1:1. The selected fractions were collected and evaporated, the residue was taken up with ethyl acetate and the resulting solid was crystallized from ethanol, to give the title compound as a white powder, m.p. 225°-227° C., (decomp.).

後処理

  1. stirringstirring
  2. waitwas prolonged at room temperature overnight
  3. customAfter evaporation under reduced pressure
  4. customthe residue was chromatographed on a silica gel column
  5. washeluting with dichloromethane/methanol 1:1
  6. customThe selected fractions were collected
  7. customevaporated
  8. customthe resulting solid was crystallized from ethanol

出典と根拠

ORDレコード
ord-8bd97c6e19a4404ca2ced4eba6826bdc
出典データセット
uspto-grants-1987_10
特許番号
US04703054

反応ノート

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