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Dicyclohexylcarbodiimide → HCID 85136525、化合物

HRID 1792980
ノート
印刷プレビュー

反応式

HRID 1792980 の反応式
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH:18]=[CH:19][C:20]([OH:22])=O)[CH:9]=[C:10]([O:13][CH2:14][CH2:15][CH2:16][CH3:17])[C:11]=1[OH:12])[CH2:2][CH2:3][CH3:4].[NH2:23][CH2:24][CH2:25][C:26]1[CH:31]=[C:30]([C:32]([CH3:35])([CH3:34])[CH3:33])[C:29]([OH:36])=[C:28]([C:37]([CH3:40])([CH3:39])[CH3:38])[CH:27]=1.C1C=CC2N(O)N=NC=2C=1.C1CCC(N=C=NC2CCCCC2)CC1>CC#N>[CH2:14]([O:13][C:10]1[CH:9]=[C:8]([CH:18]=[CH:19][C:20]([NH:23][CH2:24][CH2:25][C:26]2[CH:31]=[C:30]([C:32]([CH3:33])([CH3:35])[CH3:34])[C:29]([OH:36])=[C:28]([C:37]([CH3:40])([CH3:39])[CH3:38])[CH:27]=2)=[O:22])[CH:7]=[C:6]([O:5][CH2:1][CH2:2][CH2:3][CH3:4])[C:11]=1[OH:12])[CH2:15][CH2:16][CH3:17]
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 4

HCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 104908664-(2-Aminoethyl)-2,6-di-t-butylphenolHCID 69640036HCID 69640036、化合物

生成物 1

HCID 85136525HCID 85136525、化合物収率 91.5%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

To the solution of 3-(3,5-dibutoxy-4-hydroxyphenyl)acrylic acid (130 mg, 0.421 mmol), 4-(2-aminoethyl)-2,6-di-t-butylphenol (110 mg, 0.441 mmol) and HOBT (70 mg, 0.51 mmol) in MeCN 10 ml were DCC at 0° C. After 5 minutes, the solution was stirred for 2 hours at room temperature. And then the precipitate was removed by filtering it through a celite layer and the solution was poured into CH2Cl2. The solution was washed with 2N HCl and saturated NaHCO3 solution and the water was dried over anhydrous magnesium sulfate and filtered. The obtained filtrate was vacuum concentrated to give the residue, which was purified by column chromatography (EtOAc:Hexane=1:3), yielding 208 mg (91%) of the title compound.

後処理

  1. customat 0° C
  2. customAnd then the precipitate was removed
  3. filtrationby filtering it through a celite layer
  4. additionthe solution was poured into CH2Cl2
  5. washThe solution was washed with 2N HCl and saturated NaHCO3 solution
  6. dry with materialthe water was dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give the residue, which
  10. customwas purified by column chromatography (EtOAc:Hexane=1:3)

出典と根拠

ORDレコード
ord-15ed3afbed324fc5a0787f9298282063
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07078407B2

反応ノート

読み込み中…

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