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Dimethylformamide → HCID 22116938, 화합물

HRID 355594
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인쇄 미리보기

반응식

HRID 355594 반응식
[CH3:1][C:2]1([CH3:26])[C:6](=[O:7])[N:5]([C:8]2[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[C:10]([C:16]([F:19])([F:18])[F:17])[CH:9]=2)[C:4](=[O:20])[N:3]1[CH2:21][CH2:22][CH2:23][CH2:24][OH:25].[C:27](Cl)([C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C(N(CC)CC)C.CN(C)C=O>CN(C)C1C=CN=CC=1.CCOCC.O>[O:20]=[C:4]1[N:3]([CH2:21][CH2:22][CH2:23][CH2:24][O:25][C:27]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)([C:40]2[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=2)[C:34]2[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=2)[C:2]([CH3:26])([CH3:1])[C:6](=[O:7])[N:5]1[C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[C:10]([C:16]([F:17])([F:18])[F:19])[CH:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6228DimethylformamideHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 1329814-(3-(4-Hydroxybutyl)-4,4-dimethyl-2,5-dioxo-1-imidazolidinyl)-2-(trifluoromethyl)benzonitrile

생성물 1

HCID 22116938HCID 22116938, 화합물수율 76.2%

시약·촉매·용매 3

HCID 14284
4-(Dimethylamino)pyridine
촉매
HCID 962Water용매
HCID 3283Diethyl Ether용매

반응 조건

온도
40 °C

실험 절차

370 mg of the product of Example 58, 307 mg of trityl chloride in the presence of 10 mg of 4-dimethylaminopyridine, 0.25 ml of triethylamine and 4 ml of dimethylformamide were stirred at ambient temperature for 16 hours. The mixture was heated to 40° C. for 4 hours, poured into water and extraction was carried out with ether. The extracts were washed with water and dried and the solvent was eliminated under reduced pressure. The residue was chromatographed on silica (eluant: cyclohexane--ethyl acetate 75-25) to obtain 467 mg of the expected product with a Rf=0.25.

후처리

  1. washThe extracts were washed with water
  2. customdried
  3. customThe residue was chromatographed on silica (eluant: cyclohexane--ethyl acetate 75-25)

출처 및 근거

ORD 기록
ord-5e1f7b717f3749b6b581c38ca2984e61
출처 데이터셋
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE035956

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