Water → HCID 21488274, 화합물

HRID 1974011노트

반응식

HRID 1974011 반응식
O[CH:2]1[CH2:9][CH2:8][CH:7]([OH:10])[CH:6]2[N:11]([CH3:12])[CH:3]1[CH2:4][CH2:5]2.[C:13]([C:17]1[CH:18]=[C:19]([CH2:28][C:29]([OH:31])=[O:30])[CH:20]=[C:21]([C:24]([CH3:27])([CH3:26])[CH3:25])[C:22]=1[OH:23])([CH3:16])([CH3:15])[CH3:14].[OH2:32]>C1(C)C(C)=CC=CC=1.CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4]>[C:13]([C:17]1[CH:18]=[C:19]([CH2:28][C:29]([O:31][CH:3]2[CH2:4][CH2:5][CH:6]3[N:11]([CH3:12])[CH:2]2[CH2:9][CH2:8][CH:7]3[O:10][C:29](=[O:30])[CH2:28][C:19]2[CH:20]=[C:21]([C:24]([CH3:25])([CH3:27])[CH3:26])[C:22]([OH:32])=[C:17]([C:13]([CH3:16])([CH3:15])[CH3:14])[CH:18]=2)=[O:30])[CH:20]=[C:21]([C:24]([CH3:25])([CH3:27])[CH3:26])[C:22]=1[OH:23])([CH3:16])([CH3:14])[CH3:15]

참가 물질

6

반응물 3

HCID 962WaterHCID 27751103,5-Bis(1,1-dimethylethyl)-4-hydroxybenzeneacetic acidHCID 214882869-Methyl-9-azabicyclo[4.2.1]nonane-2,5-diol

생성물 1

HCID 21488274HCID 21488274, 화합물수율 28%

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 7237O-Xylene용매

실험 절차

Under nitrogen a stirred solution of the diol mixture 2,6-dihydroxy-9-methyl-9-azabicyclo [3.3.1]nonane and 2,5-dihydroxy-9-methyl-9-azabicyclo[4.2.1]nonane (4.28 g, 0.025 mole), 3,5-di-tert-butyl-4-hydroxyphenylacetic acid (14.55 g, 0.055 mole) and titanium tetraisopropylate (0.7 ml) in 100 ml of xylene was heated under reflux for 18 hours water being removed with a Dean-Stark trap. The xylene was evaporated under reduced pressure and the residue was dissolved in ether. The ether solution was washed with water then 10% aqueous sodium hydroxide and again with water. The dried (Na2SO4) solution was crystallized from petroleum ether and then from hexane to give 4.6 g (28%) of the desired ester, m.p. 98°-100° C.

후처리

  1. customremoved with a Dean-Stark trap
  2. customThe xylene was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in ether
  4. washThe ether solution was washed with water
  5. dry with materialThe dried (Na2SO4) solution
  6. customwas crystallized from petroleum ether

출처 및 근거

ORD 기록
ord-19cc62e005ae4e4f90cdeef9a1da2de5
출처 데이터셋
uspto-grants-1976_12
특허 번호
US04000113

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