2,2'-((1-Methylethylidene)bis(cyclohexane-4,1-diyloxymethylene))bisoxirane → 2,2-Bis{4-[2-hydroxy-3-(7,7,8,9,9-pentamethyl2,4-dioxo-1,3,8-triazaspiro[4.5]dec-3-yl)propoxy]cyclohexyl}propane

HRID 972031

반응식

HRID 972031 반응식
[CH3:1][C:2]1([CH3:17])[N:13]([CH3:14])[C:12]([CH3:16])([CH3:15])[CH2:11][C:4]2([NH:8][C:7](=[O:9])[NH:6][C:5]2=[O:10])[CH2:3]1.O1CC1C[O:21][CH:22]1[CH2:27][CH2:26][CH:25]([C:28]([CH:31]2[CH2:36][CH2:35][CH:34]([O:37][CH2:38][CH:39]3[O:41][CH2:40]3)[CH2:33][CH2:32]2)([CH3:30])[CH3:29])[CH2:24][CH2:23]1>>[OH:21][CH:22]([CH2:27][N:6]1[C:5](=[O:10])[C:4]2([CH2:3][C:2]([CH3:17])([CH3:1])[N:13]([CH3:14])[C:12]([CH3:16])([CH3:15])[CH2:11]2)[NH:8][C:7]1=[O:9])[CH2:23][O:21][CH:22]1[CH2:27][CH2:26][CH:25]([C:28]([CH:31]2[CH2:32][CH2:33][CH:34]([O:37][CH2:38][CH:39]([OH:41])[CH2:40][N:6]3[C:5](=[O:10])[C:4]4([CH2:3][C:2]([CH3:17])([CH3:1])[N:13]([CH3:14])[C:12]([CH3:16])([CH3:15])[CH2:11]4)[NH:8][C:7]3=[O:9])[CH2:35][CH2:36]2)([CH3:30])[CH3:29])[CH2:24][CH2:23]1

참가 물질

3

반응물 2

HCID 1145142,2'-((1-Methylethylidene)bis(cyclohexane-4,1-diyloxymethylene))bisoxiraneHCID 204818537,7,8,9,9-Pentamethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

생성물 1

HCID 203967902,2-Bis{4-[2-hydroxy-3-(7,7,8,9,9-pentamethyl2,4-dioxo-1,3,8-triazaspiro[4.5]dec-3-yl)propoxy]cyclohexyl}propane

실험 절차

A mixture of 8 g of 7,7,8,9,9-pentamethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione and 5 g of 2,2-bis[4-(2,3-epoxypropoxy)cyclohexyl]propane was heated at 180°-200° C. for 5 hours. The reaction mixture was then purified by column chromatography through silica gel eluted with a 60:10:1 by volume mixture of ethyl acetate, ethanol and triethylamine and then by recrystallisation from ethyl acetate, giving the desired compound in the form of white crystals melting at 130°-133° C.

후처리

  1. temperaturewas heated at 180°-200° C. for 5 hours
  2. customThe reaction mixture was then purified by column chromatography through silica gel
  3. washeluted with a 60:10:1 by volume mixture of ethyl acetate, ethanol and triethylamine
  4. customby recrystallisation from ethyl acetate

출처 및 근거

ORD 기록
ord-0e42e3277a1d4944b43a1754307a4991
출처 데이터셋
uspto-grants-1979_07
특허 번호
US04162246

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