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Triethylamine → N-(1-Hydroxy-2-methylpropan-2-yl)-2-methoxybenzamide

HRID 343954
ノート
印刷プレビュー

反応式

HRID 343954 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=O.N1C=CN=N1.OC1(C=CC=CC1)C(O)=O.[OH:27][CH2:28][C:29]([NH2:32])([CH3:31])[CH3:30].C(N(CC)CC)C>C(Cl)Cl.O>[OH:27][CH2:28][C:29]([NH:32][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][CH:10]=[CH:11][C:3]=1[O:2][CH3:1])([CH3:31])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 113702-Methoxybenzoic acidHCID 118072-Amino-2-methyl-1-propanolHCID 178524978HCID 178524978、化合物

生成物 1

HCID 2764140N-(1-Hydroxy-2-methylpropan-2-yl)-2-methoxybenzamide

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

15.2 g (100 mmol) of 2-methoxy-benzoic acid are dissolved in 300 ml of methylene chloride and the solution is stirred with 14.2 g (105 mmol) of 1-hydroxy-benzoic acid triazole×1 H2O and 21.66 g (105 mmol) of N,N-dicyclohexylcarbodiimide at 0° C. The suspension thus obtained is stirred at room temperature for 0.5 hour, cooled to 0° C. again, and a solution of 9.89 g (111 mmol) of 1-hydroxy-2-methyl-2-propylamine and 12.65 g (125 mmol) of triethylamine in 300 ml of methylene chloride is added. The reaction is complete after 1 hour. The reaction mixture is washed with 1M of hydrochloric acid and saturated sodium bicarbonate solution, dried over sodium sulphate and concentrated in vacuo. The crude product is stirred with petroleum ether, filtered off with suction, subsequently rinsed with the solvent and dried under a high vacuum.

後処理

  1. customThe suspension thus obtained
  2. temperaturecooled to 0° C. again
  3. waitThe reaction is complete after 1 hour
  4. washThe reaction mixture is washed with 1M of hydrochloric acid and saturated sodium bicarbonate solution
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo
  7. stirringThe crude product is stirred with petroleum ether
  8. filtrationfiltered off with suction
  9. washsubsequently rinsed with the solvent
  10. customdried under a high vacuum

出典と根拠

ORDレコード
ord-16bdeea848164c49898119ab4d89fa42
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05863930

反応ノート

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