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Dimethylformamide → HCID 21833472, 화합물

HRID 1740860
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HRID 1740860 반응식
[OH:1][CH2:2][C:3]([N:5]([CH2:9][CH2:10][CH3:11])[CH2:6][CH2:7][CH3:8])=[O:4].CN(C)C=O.[H-].[Na+].Cl[C:20]1[C:29]2[CH2:28][CH2:27][CH2:26][CH2:25][C:24]=2[N:23]=[C:22]([C:30]2[CH:35]=[CH:34][C:33]([F:36])=[CH:32][CH:31]=2)[N:21]=1>C(Cl)(Cl)Cl>[F:36][C:33]1[CH:34]=[CH:35][C:30]([C:22]2[N:21]=[C:20]([O:1][CH2:2][C:3]([N:5]([CH2:9][CH2:10][CH3:11])[CH2:6][CH2:7][CH3:8])=[O:4])[C:29]3[CH2:28][CH2:27][CH2:26][CH2:25][C:24]=3[N:23]=2)=[CH:31][CH:32]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 138235672-Hydroxy-N,N-dipropylacetamideHCID 21833538HCID 21833538, 화합물

생성물 1

HCID 21833472HCID 21833472, 화합물수율 75%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
0 °C

실험 절차

To a mixture of 2-hydroxy-N,N-dipropylacetamide (1.8 g) and dimethylformamide (20 ml) is added sodium hydride (about 60% oily, 0.5 g) at 0 to 5° C., and the mixture is stirred at 0° C. for one hour. To the reaction mixture is added 4-chloro-2-(4-fluorophenyl)-5,6,7,8-tetrahydroquinazoline (2.0 g) at the same temperature, and the mixture is stirred at room temperature for four hours. To the mixture are added chloroform and ice-water, and the chloroform layer is collected, washed with water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (eluent; chloroform), and recrystallized from a mixture of diethyl ether and n-hexane to give the desired compound (2.2 g), m.p. 95-96° C.

후처리

  1. stirringthe mixture is stirred at room temperature for four hours
  2. customthe chloroform layer is collected
  3. washwashed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue is purified by silica gel column chromatography (eluent; chloroform)
  7. customrecrystallized from a mixture of diethyl ether and n-hexane

출처 및 근거

ORD 기록
ord-353e52fd375346099c2afea2d33c6ce6
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05972946

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