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

HRID 1380419
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HRID 1380419 반응식
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]
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참가 물질

4

반응물 2

HCID 10868DicyclohexylcarbodiimideHCID 133137911-(2-Hydroxycarbonyl-3,3,3-trifluoropropyl)-3-methylurea

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-bbd2ecfa404748ed8c51d65b861ce89c
출처 데이터셋
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04581452

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