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Dichloromethane → 2-Methylsulfanyl-4-o-tolyl-pyrimidine-5-carboxylic acid (3,5-dimethyl-benzyl)-methyl-amide

HRID 650636
ノート
印刷プレビュー

反応式

HRID 650636 の反応式
[CH3:1][S:2][C:3]1[N:8]=[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[CH3:15])[C:6]([C:16]([OH:18])=O)=[CH:5][N:4]=1.ON1C2[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=2N=N1.Cl.CN(C)[CH2:32][CH2:33][CH2:34][N:35]=[C:36]=NCC.[CH2:41](Cl)Cl>>[CH3:41][C:28]1[CH:23]=[C:33]([CH:32]=[C:26]([CH3:25])[CH:27]=1)[CH2:34][N:35]([CH3:36])[C:16]([C:6]1[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[CH3:15])=[N:8][C:3]([S:2][CH3:1])=[N:4][CH:5]=1)=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 6344Dichloromethane2 回HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 217124342-Methylsulfanyl-4-o-tolyl-pyrimidine-5-carboxylic acid

生成物 1

HCID 537884882-Methylsulfanyl-4-o-tolyl-pyrimidine-5-carboxylic acid (3,5-dimethyl-benzyl)-methyl-amide収率 82%

実験手順

To a solution of 2.60 g (9.99 mmol) 2-methylsulfanyl-4-o-tolyl-pyrimidine-5-carboxylic acid in 70 ml CH2Cl2 2.78 ml (19.98 mmol) triethylamine, 1.34 g (9.99 mmol) 1-hydroxybenzotriazole and 1.91 g (9.99 mmol) N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride 1.78 g (11.99 mmol) (3,5-dimethoxy-benzyl)-methyl-amine were added. The reaction mixture was stirred for 16 hrs. The reaction mixture was diluted with 100 ml CH2Cl2, washed with 100 ml 0.5N HCl and 100 ml H2O. The aqueous layers were backextracted with 100 ml CH2Cl2. The combined organic layers were dried (MgSO4), filtered and evaporated. The residue was purified by chromatography (SiO2, CH2Cl2/MeOH 40:1) to give 3.20 g (82%) 2-methylsulfanyl-4-o-tolyl-pyrimidine-5-carboxylic acid (3,5-dimethyl-benzyl)-methyl-amide as a pale yellow oil, MS (EI): 391 (M+).

後処理

  1. washwashed with 100 ml 0.5N HCl and 100 ml H2O
  2. dry with materialThe combined organic layers were dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated
  5. customThe residue was purified by chromatography (SiO2, CH2Cl2/MeOH 40:1)

出典と根拠

ORDレコード
ord-f7171ddf1ff44aaf84d1d91055a8d721
出典データセット
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06274588B1

反応ノート

読み込み中…

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