Dimethylformamide → HCID 9951306、化合物

HRID 1265043ノート

反応式

HRID 1265043 の反応式
[O:1]=[C:2]1[NH:6][C:5](=[O:7])[CH:4]([CH2:8][C:9]2[CH:10]=[CH:11][C:12]([O:18][CH3:19])=[C:13]([CH:17]=2)[C:14]([OH:16])=O)[S:3]1.[N:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:26][NH2:27].Cl.CN(C)CCCN=C=NCC.CN(C)C=O>O>[N:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:26][NH:27][C:14](=[O:16])[C:13]1[CH:17]=[C:9]([CH2:8][CH:4]2[S:3][C:2](=[O:1])[NH:6][C:5]2=[O:7])[CH:10]=[CH:11][C:12]=1[O:18][CH3:19]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 195092-PyridinemethanamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 9943613HCID 9943613、化合物

生成物 1

HCID 9951306HCID 9951306、化合物収率 20%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5-[(2,4-Dioxothiazolidin-5-yl)methyl]-2-methoxybenzoic acid (282 mg, 1.00 mmol), 2-picolylamine (114 mg, 1.05 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (230 mg, 1.20 mmol) and N,N-dimethylformamide (5 mL) were mixed and stirred for 5.5 hours at room temperature, which was then allowed to stand overnight. After water was added to the reaction mixture, this was made acidic and extracted with ethyl acetate. The extracted solution was dried and then concentrated. The residue was recrystallized from acetonitrile to obtain 73.7 mg (20%) of the title compound as colorless crystals.

後処理

  1. waitto stand overnight
  2. extractionextracted with ethyl acetate
  3. customThe extracted solution was dried
  4. concentrationconcentrated
  5. customThe residue was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-beea16d6ea6d467d8c4e3251ca736dc0
出典データセット
uspto-grants-2003_04
特許番号
US06545026B1

反応ノート

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