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Dicyclohexylcarbodiimide → HCID 21976135、化合物

HRID 11734
ノート
印刷プレビュー

反応式

HRID 11734 の反応式
[C:1]1([CH3:21])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[N:9](C1C=CC=CC=1)[C:10](=[O:14])[C:11]([OH:13])=O.ON1C2C=CC=CC=2N=N1.C1(N=C=NC2CCCCC2)CCCCC1.[NH2:47][C:48]1[CH:53]=[C:52]([CH3:54])[CH:51]=[C:50]([C:55]([CH3:58])([CH3:57])[CH3:56])[C:49]=1[OH:59]>C1COCC1>[C:3]1([CH3:8])[CH:4]=[C:5]([CH3:7])[CH:6]=[C:1]([CH3:21])[C:2]=1[NH:9][C:10](=[O:14])[C:11]([NH:47][C:48]1[CH:53]=[C:52]([CH3:54])[CH:51]=[C:50]([C:55]([CH3:57])([CH3:56])[CH3:58])[C:49]=1[OH:59])=[O:13]
参加物反応条件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 5964582-Amino-6-tert-butyl-4-methyl-phenolHCID 21976145HCID 21976145、化合物

生成物 1

HCID 21976135HCID 21976135、化合物収率 76%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

反応条件

温度
0 °C

実験手順

N-(Mesityl)-oxanilic acid (2.15 g, 10.4 mmol, 1.0 eq), prepared according to the synthesis method described in Example 5, and 1-hydroxybenzotriazole (2.39 g, 15.6 mmol, 1.5 eq) were added to an oven dried, two-necked flask, forming a solution. THF (100 ml) was then added and the solution was cooled to 0° C. 1,3-dicyclohexylcarbodiimide (1 M in CH2Cl2) (12.5 ml, 12.5 mmol, 1.2 eq) was then added to the solution. The solution was then allowed to stir at 0° for one hour. During this time, a white precipitate formed. 2-amino-4-methyl-6-tert-butylphenol (1.863 g, 10.4 mmol, 1.0 eq), prepared according to the synthesis method described in Example 6, was then added to the suspension. The suspension was then allowed to stir overnight. The next day, the solvent was removed under reduced pressure, and ethyl acetate was added. The resulting suspension was then filtered to remove the solid. The filtrate was washed with 10% citric acid solution (2×50 ml), 5% NaHCO3 (2×50 ml) and brine (50 ml). It was dried over MgSO4, and the solvent was removed under reduced pressure, leaving a solid which was recrystallized from hexane to give the product as a white solid (2.92 g, 7.9 mmol, 76% yield). 1H NMR (300 MHz, CDCl3) δ 9.55 (s, 1H), 8.77 (s, 1H), 7.84 (s, 1H), 7.05 (d, J=1.8 Hz, 1H), 6.92 (m, 3H), 2.30 (s, 3H), 2.28 (s, 3H), 2.22 (s, 6H), 1.45 (s, 9H); 13C NMR (75 MHz, CDCl3) δ 158.5, 157.4, 146.2, 140.6, 138.1, 134.9, 129.9, 129.6, 129.4, 126.9, 124.9, 121.4, 35.3, 30.0, 21.2, 21.0, 18.5. Anal. Calcd for C22H28N2O3: C, 71.71; H, 7.66; N, 7.60. Found: C, 72.01; H, 8.03; N, 7.36.

後処理

  1. customaccording to the synthesis method
  2. additionwere added to an oven
  3. customdried
  4. customtwo-necked flask, forming a solution
  5. customDuring this time, a white precipitate formed
  6. customaccording to the synthesis method
  7. additionwas then added to the suspension
  8. stirringto stir overnight
  9. customThe next day, the solvent was removed under reduced pressure, and ethyl acetate
  10. additionwas added
  11. filtrationThe resulting suspension was then filtered
  12. customto remove the solid
  13. washThe filtrate was washed with 10% citric acid solution (2×50 ml), 5% NaHCO3 (2×50 ml) and brine (50 ml)
  14. dry with materialIt was dried over MgSO4
  15. customthe solvent was removed under reduced pressure
  16. customleaving a solid which
  17. customwas recrystallized from hexane

出典と根拠

ORDレコード
ord-5d6f768b9327470e9be2d5fc1997a9f5
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07098278B2

反応ノート

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