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Water → HCID 86740382, 화합물

HRID 464764
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HRID 464764 반응식
O.[CH3:2][C:3]1O[C:5]([CH3:14])=[CH:6][C:7](=[O:13])[C:8]=1[C:9]([O:11][CH3:12])=[O:10].[NH2:15][CH:16]1[CH2:21][C:20]([CH3:23])([CH3:22])[NH:19][C:18]([CH3:25])([CH3:24])[CH2:17]1>C1(C)C=CC=CC=1>[CH3:2][C:3]1[N:15]([CH:16]2[CH2:17][C:18]([CH3:25])([CH3:24])[NH:19][C:20]([CH3:23])([CH3:22])[CH2:21]2)[C:5]([CH3:14])=[CH:6][C:7](=[O:13])[C:8]=1[C:9]([O:11][CH3:12])=[O:10]
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반응물 3

HCID 962WaterHCID 375244-Amino-2,2,6,6-tetramethylpiperidineHCID 122813714H-Pyran-3-carboxylic acid, 2,6-dimethyl-4-oxo-, methyl ester2회

생성물 1

HCID 86740382HCID 86740382, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A 500 ml, 3-neck, round-bottom flask is equipped with a mechanical stirrer, thermometer and a Dean-Stark water trap topped with a water cooled condenser. The flask is charged with a mixture of 45.5 g (0.25 moles) of the methyl 2,6-dimethyl-4-oxopyran-3-carboxylate prepared as described above, 39.1 g (0.25 m) 4-amino-2,2,6,6-tetramethylpiperidine, and 300 ml toluene. The stirred mixture in the flask is heated to boiling by means of an oil bath and the water formed during the reaction is collected in the trap. After 4 hours of reflux a total of 3.8 ml water is collected and the flask and its contents are cooled to room temperature. The toluene is removed by means of a rotary evaporator. On standing and cooling the residue deposits crystals of the title product which are further purified by fractional crystallization.

후처리

  1. customA 500 ml, 3-neck, round-bottom flask is equipped with a mechanical stirrer
  2. customprepared
  3. temperatureThe stirred mixture in the flask is heated
  4. customto boiling by means of an oil bath
  5. customis collected in the trap
  6. temperatureAfter 4 hours of reflux a total of 3.8 ml water
  7. customis collected
  8. customThe toluene is removed by means of a rotary evaporator
  9. temperaturecooling the residue deposits crystals of the title product which
  10. customare further purified by fractional crystallization

출처 및 근거

ORD 기록
ord-b91e894fc53448c599b901580aba0957
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04548973

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