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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → 4-Oxazolecarboxylic acid, 5-(4-chlorophenyl)-, methyl ester

HRID 2092243
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반응식

HRID 2092243 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[N:11]([CH2:14][C:15]([O:17][CH3:18])=[O:16])=[C:12]=O.C(N(CC)CC)C>C1COCC1>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]2[O:7][CH:12]=[N:11][C:14]=2[C:15]([O:17][CH3:18])=[O:16])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 85014-Chlorobenzoyl chlorideHCID 2769479Methyl 2-isocyanatoacetate

생성물 1

HCID 118463424-Oxazolecarboxylic acid, 5-(4-chlorophenyl)-, methyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1.40 g (8.00 mmol) of 4-chlorobenzoyl chloride, 1.00 g (10.09 mmol) of methyl isocyanatoacetate and 5.9 ml (42.39 mmol) of triethylamine are dissolved in 15 ml of dry THF and stirred at RT for 48 h. The solvent is then removed on a rotary evaporator. The residue is taken up in 20 ml of ethyl acetate and washed once with 5 ml of water. The organic phase is dried over magnesium sulfate and the solvent is removed on a rotary evaporator. The residue is suspended in 10 ml of cyclohexane and filtered off. It is then recrystallized from about 10 ml of methanol. This gives needle-shaped crystals which are dried in a drying cabinet at 50° C. A further product fraction is obtained by reprecipitation after recrystallization.

후처리

  1. customThe solvent is then removed on a rotary evaporator
  2. washwashed once with 5 ml of water
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. customthe solvent is removed on a rotary evaporator
  5. filtrationfiltered off
  6. customIt is then recrystallized from about 10 ml of methanol
  7. customThis gives needle-shaped crystals which are dried in a drying cabinet at 50° C
  8. customA further product fraction is obtained by reprecipitation
  9. customafter recrystallization

출처 및 근거

ORD 기록
ord-1115645405724ff78f54f0c1c34196a0
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08440700B2

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