Squaric acid → HCID 178448829, 화합물

HRID 485733

반응식

HRID 485733 반응식
[CH2:1]([NH:5][CH:6]1[CH2:11][C:10]([CH3:13])([CH3:12])[NH:9][C:8]([CH3:15])([CH3:14])[CH2:7]1)[CH2:2][CH2:3][CH3:4].[C:16]1(O)[C:20](=[O:21])[C:18](=O)[C:17]=1[OH:22]>C(C(CCCC)CO)C>[CH2:1]([N:5]([C+:16]1[C:17]([O-:22])=[C:18]([N:5]([CH:6]2[CH2:7][C:8]([CH3:15])([CH3:14])[NH:9][C:10]([CH3:12])([CH3:13])[CH2:11]2)[CH2:1][CH2:2][CH2:3][CH3:4])[C+:20]1[O-:21])[CH:6]1[CH2:7][C:8]([CH3:14])([CH3:15])[NH:9][C:10]([CH3:13])([CH3:12])[CH2:11]1)[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 17913Squaric acidHCID 118285n-Butyl-2,2,6,6-tetramethyl-4-piperidinamine

생성물 1

HCID 178448829HCID 178448829, 화합물수율 88.2%

시약·촉매·용매 1

HCID 77202-Ethylhexanol용매

실험 절차

Under agitation, 392.9 g (1.85 moles) of 4-n-butylamino-2,2,6,6-tetramethylpiperidine, 10.0 g (0.0877 mole) of quadratic acid, and 150 cc of 2-ethylhexanol were heated to boiling under reflux in a 1-liter agitated flask with water trap; s temperature rose from 205° to 217° C., and 2.8 cc of water was removed from the cycle. The reaction solution was then distilled. The residue was boiled with petroleum ether. After cooling, vacuum-filtering, and drying, 38.9 g was obtained (88.2% yield), mp 151°-152° C. Extinction (g/l.cm) at 278 nm: 25; at 335 nm: 83.

후처리

  1. temperatureunder reflux in a 1-liter
  2. customrose from 205° to 217° C.
  3. custom2.8 cc of water was removed from the cycle
  4. distillationThe reaction solution was then distilled
  5. temperatureAfter cooling
  6. filtrationvacuum-filtering
  7. customdrying
  8. custom38.9 g was obtained (88.2% yield), mp 151°-152° C

출처 및 근거

ORD 기록
ord-90b8d0c5bce94e7da822fedaadf8c796
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04537924

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