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2-(2-(2-Azidoethoxy)ethoxy)ethanol → Mono-2-(2-(2-(4-(methylene)-1H-1,2,3-triazol-1-yl)ethoxy)ethoxy)ethanol-curcumin

HRID 452022
ノート
印刷プレビュー

反応式

HRID 452022 の反応式
C([CH:4]([C:18](/[CH:20]=[CH:21]/[C:22]1[CH:30]=[C:27]([O:28][CH3:29])[C:25]([OH:26])=[CH:24][CH:23]=1)=[O:19])[C:5](=[O:17])/[CH:6]=[CH:7]/[C:8]1[CH:9]=[C:10]([C:13]([OH:16])=[CH:14][CH:15]=1)[O:11][CH3:12])C#C.[N:31]([CH2:34][CH2:35][O:36][CH2:37][CH2:38][O:39][CH2:40][CH2:41][OH:42])=[N+:32]=[N-:33].O=[C:44]1O[C@H]([C@H](CO)O)[C:47]([O-])=[C:45]1O.[Na+]>CC(O)(C)C.C(Cl)(Cl)Cl.O.CC([O-])=O.CC([O-])=O.[Cu+2]>[CH3:29][O:28][C:27]1[C:25]([OH:26])=[CH:24][CH:23]=[C:22](/[CH:21]=[CH:20]/[C:18]([CH2:4][C:5](/[CH:6]=[CH:7]/[C:8]2[CH:9]=[C:10]([O:11][CH3:12])[C:13]([OH:16])=[CH:14][CH:15]=2)=[O:17])=[O:19])[CH:30]=1.[CH2:44]=[C:45]1[CH2:47][N:31]([CH2:34][CH2:35][O:36][CH2:37][CH2:38][O:39][CH2:40][CH2:41][OH:42])[N:32]=[N:33]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 110084382-(2-(2-Azidoethoxy)ethoxy)ethanolHCID 23667548Sodium AscorbateHCID 88539422Mono-Propargyl Curcumin

生成物 1

HCID 131730719Mono-2-(2-(2-(4-(methylene)-1H-1,2,3-triazol-1-yl)ethoxy)ethoxy)ethanol-curcumin収率 26%

試薬・触媒・溶媒 4

HCID 8895Cupric acetate触媒
HCID 962
Water
溶媒
HCID 6212Chloroform溶媒
HCID 6386tert-Butanol溶媒

実験手順

To a stirred solution of Mono-Propargyl Curcumin 5 (63 mg, 0.16 mmol) and 2-(2-(2-azidoethoxy)ethoxy)ethanol (46 mg, 0.26 mmol) in tBuOH (1.1 mL) and CHCl3 (0.3 mL) was added a prepared solution of Cu(OAc)2 (8 mg, 0.03 mmol) and sodium ascorbate (13 mg, 0.07 mmol) in H2O (1.3 mL). After vigorous stirring overnight the solvent was removed under vacuum. The mixture was dissolved in CHCl3, washed with H2O and the organic phase was separated, dried over Na2SO4 and evaporated. Purification was performed by column chromatography, eluting with CH2Cl2-CH2Cl2: MeOH 98:2. Yield 26%. NMR NMR 1H (CDCl3), δ (ppm): 3.55-3.60 (m, 8H); 3.72-3.72 (t, 3H); 3.87-3.94 (m, 8H); 4.54-4.55 (t, 2H); 5.80 (s, 1H); 6.07 (s, 1H); 6.46-6.50 (dd, 2H); 6.92-6.94 (d, 1H); 7.05-7.12 (m, 5H); 7.56-7.60 (q, 2H); 7.92 (s, 1H).). MS (ESI) calcd. for C30H35N3O9: 581.61. Found: 582.3 [M+H]+, 604.3 [M++Na], 620.3 [M++K].

後処理

  1. customwas removed under vacuum
  2. dissolutionThe mixture was dissolved in CHCl3
  3. washwashed with H2O
  4. customthe organic phase was separated
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. customPurification
  8. washeluting with CH2Cl2-CH2Cl2

出典と根拠

ORDレコード
ord-b47b36a534c54e639febfd0283672cb1
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08487139B2

反応ノート

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