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Dicyclohexylcarbodiimide → 3-Methyl-5-(trifluoromethyl)dihydropyrimidine-2,4(1H,3H)-dione

HRID 1380419
ノート
印刷プレビュー

反応式

HRID 1380419 の反応式
C1CCC(N=C=NC2CCCCC2)CC1.[OH:16][C:17]([CH:19]([C:26]([F:29])([F:28])[F:27])[CH2:20][NH:21][C:22]([NH:24][CH3:25])=[O:23])=O>CN(C=O)C>[CH3:25][N:24]1[C:17](=[O:16])[CH:19]([C:26]([F:29])([F:28])[F:27])[CH2:20][NH:21][C:22]1=[O:23]
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 10868DicyclohexylcarbodiimideHCID 133137911-(2-Hydroxycarbonyl-3,3,3-trifluoropropyl)-3-methylurea

生成物 1

HCID 130049793-Methyl-5-(trifluoromethyl)dihydropyrimidine-2,4(1H,3H)-dione収率 94%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of DCC (428 mg; 2.1 mmoles) in DMF (1 ml) was added dropwise to a solution of 1-(2-hydroxycarbonyl-3,3,3-trifluoropropyl)-3-methylurea (428 mg; 2.0 mmoles) obtained above in DMF (2 ml). The mixture was stirred for 1 hour, and the precipitated solid was filtered off and washed with ethyl acetate. The solvents were evaporated under reduced pressure from the combined filtrates. The residue was purified by a column chromatography on silica gel (ethyl acetate:chloroform=1:1) to give 368 mg (yield: 94%) of 3-methyl-5-trifluoromethyl-5,6-dihydrouracil (OF-2).

後処理

  1. filtrationthe precipitated solid was filtered off
  2. washwashed with ethyl acetate
  3. customThe solvents were evaporated under reduced pressure from the combined filtrates
  4. customThe residue was purified by a column chromatography on silica gel (ethyl acetate:chloroform=1:1)

出典と根拠

ORDレコード
ord-bbd2ecfa404748ed8c51d65b861ce89c
出典データセット
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04581452

反応ノート

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