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Sodium hydride → HCID 68642095, 화합물

HRID 1498948
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HRID 1498948 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[S:10][C:11]([C:15]([O:20][CH3:21])([O:18][CH3:19])[CH2:16][OH:17])=[C:12]([CH3:14])[N:13]=1.[CH3:22][O:23][C:24]1[CH:31]=[CH:30][C:27]([CH2:28]Cl)=[CH:26][CH:25]=1.[H-].[Na+]>CN(C)C=O>[CH3:21][O:20][C:15]([C:11]1[S:10][C:9]([C:3]2[CH:4]=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=2[CH3:1])=[N:13][C:12]=1[CH3:14])([O:18][CH3:19])[CH2:16][O:17][CH2:28][C:27]1[CH:30]=[CH:31][C:24]([O:23][CH3:22])=[CH:25][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 699934-Methyloxybenzyl chlorideHCID 68642113HCID 68642113, 화합물

생성물 1

HCID 68642095HCID 68642095, 화합물수율 64.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To N,N-dimethylformamide (2 ml), 2-[2-(2,4-dimethylphenyl)-4-methylthiazol-5-yl]-2,2-dimethoxyethanol (100 mg) prepared in the Step 31-1-2 and 4-methoxybenzyl chloride (61 mg) were added, and 60% sodium hydride suspension in oil (20 mg) was added thereto under an argon atmosphere. Then, the mixture was stirred at a room temperature for 4 hours. Ice water was added to the reaction solution, and then the mixture was subjected to extraction with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and then concentrated under a reduced pressure. The residue was purified by thin-layer chromatography (hexane:ethyl acetate=3:1) to give the title compound (90 mg, 64%).

후처리

  1. additionwere added
  2. extractionthe mixture was subjected to extraction with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under a reduced pressure
  5. customThe residue was purified by thin-layer chromatography (hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-67eab2ab8c65418092181b1f499b25c7
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09200008B2

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