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1,4-Dihydroxy-2,2,6,6-tetramethylpiperidine → HCID 54127819, 화합물

HRID 1422186
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HRID 1422186 반응식
[OH:1][N:2]1[C:7]([CH3:9])([CH3:8])[CH2:6][CH:5]([OH:10])[CH2:4][C:3]1([CH3:12])[CH3:11].C[O:14][CH2:15][CH2:16][O:17][CH2:18][C:19]([O:21][CH3:22])=O>CCCCCCC>[CH3:22][O:21][CH2:19][CH2:18][O:17][CH2:16][C:15]([O:10][CH:5]1[CH2:6][C:7]([CH3:8])([CH3:9])[N:2]([OH:1])[C:3]([CH3:12])([CH3:11])[CH2:4]1)=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 53951,4-Dihydroxy-2,2,6,6-tetramethylpiperidineHCID 28661Methyl 2-(2-methoxyethoxy)acetate

생성물 1

HCID 54127819HCID 54127819, 화합물

시약·촉매·용매 1

HCID 8900Heptane용매

실험 절차

34.4 grams of 1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine, 29.6 grams of methyl 2-methoxyethoxyacetate and 300 mL of heptane are transferred to a 500 mL 3-necked, round-bottomed flask equipped with a mechanical stirrer, Dean-Stark trap and condenser. Trace amounts of water are removed by azeotropic distillation. 0.25 mL of tetraisopropyl orthotitanate is added to the reaction mixture. The reaction mixture is refluxed for six hours and the liberated methanol is collected in the Dean-Stark trap. The reaction mixture is allowed to cool and is then partitioned between 300 mL of ethyl acetate and 300 mL of water. The phases are separated and the organic phase is washed with water and dried over anhydrous magnesium sulfate. Evaporation of the solvent leaves the title compound as a red oil.

후처리

  1. customround-bottomed flask equipped with a mechanical stirrer
  2. customTrace amounts of water are removed by azeotropic distillation
  3. addition0.25 mL of tetraisopropyl orthotitanate is added to the reaction mixture
  4. temperatureThe reaction mixture is refluxed for six hours
  5. customthe liberated methanol is collected in the Dean-Stark trap
  6. temperatureto cool
  7. customis then partitioned between 300 mL of ethyl acetate and 300 mL of water
  8. customThe phases are separated
  9. washthe organic phase is washed with water
  10. dry with materialdried over anhydrous magnesium sulfate
  11. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-649e83a046124b658e206c8d83468b5b
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06080864

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