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Triethylamine → 4-(1-(3-(Trifluoromethyl)phenyl)-2,5-dioxo-1,2,3,4,5,6,7,8-octahydroquinazolin-4-yl)-3-(methylsulfonyl)benzonitrile

HRID 59650
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HRID 59650 반응식
Cl.[NH2:2][CH:3]([C:16]1[C:21](=[O:22])[CH2:20][CH2:19][CH2:18][C:17]=1[NH:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([C:30]([F:33])([F:32])[F:31])[CH:25]=1)[C:4]1[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[CH:6][C:5]=1[S:12]([CH3:15])(=[O:14])=[O:13].[C:34](N1C=CN=C1)(N1C=CN=C1)=[O:35].C(N(CC)CC)C>C(#N)C>[O:35]=[C:34]1[NH:2][CH:3]([C:4]2[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[CH:6][C:5]=2[S:12]([CH3:15])(=[O:14])=[O:13])[C:16]2[C:21](=[O:22])[CH2:20][CH2:19][CH2:18][C:17]=2[N:23]1[C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([C:30]([F:33])([F:31])[F:32])[CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 118692887HCID 118692887, 화합물2회

생성물 1

HCID 867323284-(1-(3-(Trifluoromethyl)phenyl)-2,5-dioxo-1,2,3,4,5,6,7,8-octahydroquinazolin-4-yl)-3-(methylsulfonyl)benzonitrile

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 4-{amino-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-3-methanesulfonyl-benzonitrile hydrochloride (INTERMEDIATE 17, 529 mg, 0.95 mmol) in acetonitrile (5.0 mL) is added 1,1′-carbonyldiimidazole (192 mg, 1.19 mmol) and triethylamine (33 μL, 0.24 mmol). After stirring at room temperature over night, the reaction mixture is concentrated under reduced pressure. The residue is treated with water and the precipitate is filtered off, washed with water and dried. Yield: 468 mg. ESI mass spectrum: [M+H]+=490; Retention time HPLC: 0.57 min (X012_S01).

후처리

  1. concentrationthe reaction mixture is concentrated under reduced pressure
  2. additionThe residue is treated with water
  3. filtrationthe precipitate is filtered off
  4. washwashed with water
  5. customdried
  6. custom0.57 min (X012_S01)

출처 및 근거

ORD 기록
ord-2d2423e24a2d4650854a7e68f14f7cc4
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09440930B2

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