Nitrogen → 3,6-Dimethyl-3-octanol

HRID 275642

반응식

HRID 275642 반응식
[CH3:1][C:2]([C:4]1[CH:9]=CC=[C:6](C(N=C=O)(C)C)[CH:5]=1)=C.[C:16]([O:20]CC)(=O)[CH:17]=[CH2:18].[C:23](OC)(=O)C(C)=C.C(OOC(C)(C)C)(=O)C1C=CC=CC=1.CC(O[Hg]C1C=CC=CC=1)=O.N#N>>[CH3:1][CH2:2][CH:4]([CH2:5][CH2:6][C:16]([OH:20])([CH2:17][CH3:18])[CH3:23])[CH3:9]

참가 물질

7

반응물 6

HCID 947NitrogenHCID 6658Methyl MethacrylateHCID 8821Ethyl AcrylateHCID 11966tert-Butyl peroxybenzoateHCID 6041521-(1-Isocyanato-1-methylethyl)-3-(1-methylethenyl)benzeneHCID 16682730Phenylmercuric Acetate

생성물 1

HCID 90273,6-Dimethyl-3-octanol

반응 조건

온도
40 °C

실험 절차

30 g of M-TMI (M-TMI is 1-(1-isocyanato-1-methyl)ethyl-3-(1-methyl)ethenyl benzene, from Cytec industries), 5 g of ethyl acrylate, 15 g of methyl methacrylate and 8 g of t-butyl peroxybenzoate were heated to 120° C. in 232 g of Arcosolve PMAcetate (propylene glycol methyl ether acetate from Arco Chemicals) in a N2 purge. Then a mixture of 90 g of m-TMI, 15 g of ethyl acrylate, 45 g of methyl methacrylate, 16 g of t-butyl peroxybenzoate (Aldrich Chemicals) was added over 2 hours. After the addition was complete, an additional 8 g of t-butyl peroxybenzoate was added in two equal portions. The reaction was completed to theoretical % non-volatiles (50%) in 7 hrs. Then a partial batch of this solution (164.54 g), containing free —NCO groups of m-TMI, was further reacted with p-aminophenol (22.25 g) at 1:1 equivalent ratio. The reaction was monitored by IR-spectroscopy for disappearance of —NCO group at 2275 cm−1 and was completed by heating to 40° C. The product (AR-1), terpolymer of ethyl acrylate, methyl methacrylate and the urea adduct of m-TMI/p-aminophenol, was precipitated in powder form using water/ice, filtered and dried at room temperature. The product terpolymer AR-1 had the following structure:

후처리

  1. custompurge
  2. additionThen a mixture of 90 g of m-TMI, 15 g of ethyl acrylate, 45 g of methyl methacrylate, 16 g of t-butyl peroxybenzoate (Aldrich Chemicals)
  3. additionwas added over 2 hours
  4. additionAfter the addition
  5. additionan additional 8 g of t-butyl peroxybenzoate was added in two equal portions
  6. customin 7 hrs
  7. additionThen a partial batch of this solution (164.54 g), containing free —NCO groups of m-TMI
  8. customwas further reacted with p-aminophenol (22.25 g) at 1
  9. customThe product (AR-1), terpolymer of ethyl acrylate, methyl methacrylate and the urea adduct of m-TMI/p-aminophenol, was precipitated in powder form
  10. filtrationfiltered
  11. customdried at room temperature

출처 및 근거

ORD 기록
ord-170567226f53441cbf19ca794ecc20aa
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06352811B1

연결된 노트

불러오는 중…