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1,1'-Carbonyldiimidazole → Isatoic Anhydride

HRID 557455
ノート
印刷プレビュー

反応式

HRID 557455 の反応式
[C:1]([N:8]1[CH:12]=[CH:11]N=C1)(N1C=CN=C1)=[O:2].N[C:14]1[CH:22]=[CH:21]C(CN(C=O)C)=C[C:15]=1[C:16]([OH:18])=[O:17]>CN(C)C=O>[C:15]12[C:12](=[CH:11][CH:21]=[CH:22][CH:14]=1)[NH:8][C:1](=[O:2])[O:18][C:16]2=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 580183122-amino-5-(N-formyl-N-methylamino-methyl)benzoic acid

生成物 1

HCID 8359Isatoic Anhydride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

There was suspended, in 7.6 mL of N,N-dimethylformamide, 1.67 g of 1,1′-carbonyl-diimidazole (CDI) and the suspension was cooled to 5° C. To this slurry, there was added 2.0 g of 2-amino-5-(N-formyl-N-methylamino-methyl)-benzoic acid to thus carry out a reaction for forming an isatoic anhydride derivative at 5° C. After the confirmation of the completion of the reaction by HPLC, 3.80 g of 4-amino-Nα-(2,6-dichlorobenzoyl)-L-phenylalanine isopropyl ester was added to the reaction system to thus carry out amidation at 60° C. overnight. After the confirmation of the completion of the reaction by HPLC, the reaction system was cooled to a temperature ranging from 25 to 50° C. followed by the addition of 3 mL of water. This solution was slowly dropwise added to another egg plant-shaped flask to which 29 mL of water had previously been added to thus form a solid material and then the separated solid was isolated through filtration under reduced pressure. After washing the solid with 20 mL of water, it was dried under reduced pressure to thus give 5.50 g of a crude product of the intended compound. To this crude product, there was added 5.5 mL of acetonitrile to obtain a uniform dispersion, 137.5 mL of 2-propanol and seed crystals were added thereto to precipitate a solid material and the slurry was stirred at 20° C. for 2 hours. The solid thus separated was isolated through filtration under reduced pressure, washed with 20 mL of 2-propanol and then dried under reduced pressure to thus give 2.60 g of the intended product as a white crystalline solid.

後処理

  1. customa reaction

出典と根拠

ORDレコード
ord-babf0da8d29d4cccafecc8e6feeb21da
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058432B2

反応ノート

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