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Water → HCID 13834639, 화합물

HRID 1732015
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HRID 1732015 반응식
[C:1]([CH:3]1[S:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]1=2)#[N:2].[CH3:17]I.[H-].[Na+].O>CN(C)C=O>[C:1]([C:3]1([CH3:17])[S:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]1=2)#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 13672817HCID 13672817, 화합물

생성물 1

HCID 13834639HCID 13834639, 화합물수율 75%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of 6-cyano-6H-dibenzo[b,d]thiopyran (4.5 g; 0.02 mol) and CH3I (28.4 g; 0.2 mol) in 100 ml of dimethylformamide, 50% NaH (1.5 g; 0.03 mol) was added in small portions. After 16 hours at room temperature the mixture was poured into water and extracted with diethyl ether. The organic phase was washed with water and dried over Na2SO4. Evaporation of the solvent gave 6-cyano-6-methyl-6H-dibenzo[b,d]thiopyran (3.58 g; 0.015 mol; yield 75%).

후처리

  1. extractionextracted with diethyl ether
  2. washThe organic phase was washed with water
  3. dry with materialdried over Na2SO4
  4. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-972393a8f8b84449a4c54ecd797b9d4e
출처 데이터셋
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04624949

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