Triethylamine → HCID 20163719, 화합물

HRID 256363

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HRID 256363 반응식
[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]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 61140Butyl chloroformateHCID 31466872-(2-Oxopyrrolidin-1-yl)acetic acidHCID 21279295HCID 21279295, 화합물

생성물 1

HCID 20163719HCID 20163719, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-45569acc942d413f8c9274721a09a574
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04703054

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