Triethylamine → HCID 20163719、化合物

HRID 256363ノート

反応式

HRID 256363 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([CH3:33])[NH:31][C:30](=[O:32])[CH2:29][NH:28]1>CN(C)C=O>[CH3:26][C:27]1([CH3:33])[NH:31][C:30](=[O:32])[CH2:29][N:28]1[C:8](=[O:10])[CH2:7][N:3]1[CH2:4][CH2:5][CH2:6][C:2]1=[O:1]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 61140Butyl chloroformateHCID 31466872-(2-Oxopyrrolidin-1-yl)acetic acidHCID 21279295HCID 21279295、化合物

生成物 1

HCID 20163719HCID 20163719、化合物

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 (2.2 g) and triethylamine (2.15 ml) in dimethylformamide (10 ml) was treated dropwise while stirring with butyl chloroformate (1.95 ml). After stirring at 0° C. for 30 minutes, 2,2-dimethyl-4-imidazolidinone (1.75 g) was added at once, and stirring was continued 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 to give an oil which was washed twice with ethyl acetate. The residue was crystallized from ethyl acetate, to give the title compound as a white powder, m.p. 214°-217° C. (decomp.).

後処理

  1. stirringstirring
  2. waitwas continued at room temperature overnight
  3. customAfter evaporation under reduced pressure the residue
  4. customwas chromatographed on a silica gel column
  5. washeluting with dichloromethane/methanol 1:1
  6. customThe selected fractions were collected
  7. customevaporated
  8. customto give an oil which
  9. washwas washed twice with ethyl acetate
  10. customThe residue was crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-45569acc942d413f8c9274721a09a574
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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