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Methyl iodide → HCID 24947242, 화합물

HRID 1485005
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HRID 1485005 반응식
[CH:1]1([CH2:4][NH:5][S:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][C:17]=3[Cl:23])=[CH:11][C:10]=2[C:24]([F:27])([F:26])[F:25])(=[O:8])=[O:7])[CH2:3][CH2:2]1.CI.[CH2:30]([N+](CCCC)(CCCC)CCCC)CCC.[OH-].[Na+]>ClCCl.O>[CH:1]1([CH2:4][N:5]([CH3:30])[S:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][C:17]=3[Cl:23])=[CH:11][C:10]=2[C:24]([F:26])([F:27])[F:25])(=[O:7])=[O:8])[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 16028TetrabutylammoniumHCID 24948740HCID 24948740, 화합물

생성물 1

HCID 24947242HCID 24947242, 화합물수율 97%

시약·촉매·용매 2

HCID 962Water용매
HCID 6344
Dichloromethane
용매

실험 절차

To a solution of N-Cyclopropylmethyl-4-(2,4-dichloro-phenylamino)-2-trifluoromethyl-benzenesulfonamide, (256 mg. 0.58 mmol), methyl iodide (92 mg, 0.65 mmol) and tetrabutylammonium hydrosulfate (38 mg, 0.11 mmol) in 15 ml dichloromethane 3 ml 25% solution of NaOH was added and mixture was stirred for 3 hours. Water was added and mixture was washed twice with 1 N HCl and brine. After drying over sodium sulfate solvent was evaporated and crude solid used in the next stage. Yield 97%.

후처리

  1. washmixture was washed twice with 1 N HCl and brine
  2. dry with materialAfter drying over sodium sulfate solvent
  3. customwas evaporated

출처 및 근거

ORD 기록
ord-6316abcd874a415e9c945430883c7c28
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09422235B2

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