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Triethylamine → Methyl 3-[(4-methoxybenzoyl)amino]-4-[(4-tert-butylbenzoyl)amino]benzoate

HRID 395798
ノート
印刷プレビュー

反応式

HRID 395798 の反応式
[CH3:1][O:2][C:3]1[CH:22]=[CH:21][C:6]([C:7]([NH:9][C:10]2[CH:11]=[C:12]([CH:17]=[CH:18][C:19]=2[NH2:20])[C:13]([O:15][CH3:16])=[O:14])=[O:8])=[CH:5][CH:4]=1.C(#N)C.C(Cl)(Cl)Cl.C(N(CC)CC)C.[C:37]([C:41]1[CH:49]=[CH:48][C:44]([C:45](Cl)=[O:46])=[CH:43][CH:42]=1)([CH3:40])([CH3:39])[CH3:38]>C(#N)C>[CH3:1][O:2][C:3]1[CH:22]=[CH:21][C:6]([C:7]([NH:9][C:10]2[CH:11]=[C:12]([CH:17]=[CH:18][C:19]=2[NH:20][C:45](=[O:46])[C:44]2[CH:48]=[CH:49][C:41]([C:37]([CH3:39])([CH3:38])[CH3:40])=[CH:42][CH:43]=2)[C:13]([O:15][CH3:16])=[O:14])=[O:8])=[CH:5][CH:4]=1
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 8471TriethylamineHCID 743724-tert-Butylbenzoyl chlorideHCID 10732961Methyl 4-amino-3-(4-methoxybenzamido)benzoateHCID 22555007Acetonitrile chloroform

生成物 1

HCID 10742629Methyl 3-[(4-methoxybenzoyl)amino]-4-[(4-tert-butylbenzoyl)amino]benzoate収率 81%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

A solution of methyl 3-[(4-methoxybenzoyl)amino]-4-aminobenzoate (0.800 g, 2.67 mmol) in 1:1 acetonitrile/chloroform (100 mL) was cooled to 0° C. and treated with triethylamine (0.41 mL, 2.9 mmol), and a solution of 4-tert-butylbenzoyl chloride (0.58 mL) in acetonitrile (25 μL). The reaction mixture was allowed to warm to room temperature over 16 h, concentrated in vacuo, diluted with ethyl acetate, washed with cold dilute aqueous hydrochloric acid and cold saturated aqueous sodium bicarbonate solution. The organic layer was dried (magnesium sulfate), filtered, and concentrated in vacuo. Crystallization of the residue from methylene chloride/hexane provided 1.0 g (81%) of the title compound.

後処理

  1. concentrationconcentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. washwashed with cold dilute aqueous hydrochloric acid and cold saturated aqueous sodium bicarbonate solution
  4. dry with materialThe organic layer was dried (magnesium sulfate)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customCrystallization of the residue from methylene chloride/hexane

出典と根拠

ORDレコード
ord-c33f813b740a4c058244aab64be9211f
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06605626B2

反応ノート

読み込み中…

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