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Water → HCID 21488274、化合物

HRID 1974011
ノート
印刷プレビュー

反応式

HRID 1974011 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 21488274HCID 21488274、化合物収率 28%

試薬・触媒・溶媒 2

HCID 11026Titanium isopropoxide触媒
HCID 7237
O-Xylene
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-19cc62e005ae4e4f90cdeef9a1da2de5
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04000113

反応ノート

読み込み中…

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