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Acrolein → 3-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]thio]propanal

HRID 484171
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HRID 484171 반응식
[CH3:1][C:2]([C:5]1[CH:10]=[C:9]([SH:11])[CH:8]=[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:6]=1[OH:16])([CH3:4])[CH3:3].[CH:17]([CH:19]=[CH2:20])=[O:18].C(N(CC)CC)C>CO>[CH3:4][C:2]([C:5]1[CH:10]=[C:9]([S:11][CH2:20][CH2:19][CH:17]=[O:18])[CH:8]=[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:6]=1[OH:16])([CH3:1])[CH3:3]
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참가 물질

5

반응물 3

HCID 7847AcroleinHCID 8471TriethylamineHCID 703702,6-Di-tert-butyl-4-mercaptophenol

생성물 1

HCID 140118163-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]thio]propanal

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2,6-bis(1,1-Dimethylethyl)-4-mercaptophenol (36.4 g, 0.15 mole) was dissolved in methanol (250 ml) in a 1 liter, round bottom, 3-necked flask equipped with a stirrer, gas inlet and gas outlet. The solution was flushed with argon and freshly distilled acrolein (25 g, 0.45 mole) and triethylamine (2.4 ml) were added dropwise over a one hour period and the solvent was evaporated on a rotary evaporator and the product purified by chromatography over silica, m.p. ca. 64°-65° C.

후처리

  1. customround bottom, 3-necked flask equipped with a stirrer, gas inlet and gas outlet
  2. additionwere added dropwise over a one hour period
  3. customthe solvent was evaporated on a rotary evaporator
  4. customthe product purified by chromatography over silica, m.p. ca. 64°-65° C.

출처 및 근거

ORD 기록
ord-e67ccf9c32f14dbab087b31b83f1d1a7
출처 데이터셋
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05229421

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