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Methyl iodide → HCID 178503580, 화합물

HRID 477745
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HRID 477745 반응식
[OH-].[Na+].[CH2:3]([S:10][C:11]1[N:15]=[C:14]([SH:16])[NH:13][N:12]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH3:17]I>O.ClCCl.[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1>[CH2:3]([S:10][C:11]1[N:15]=[C:14]([S:16][CH3:17])[NH:13][N:12]=1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 178527897HCID 178527897, 화합물

생성물 1

HCID 178503580HCID 178503580, 화합물수율 85.1%

시약·촉매·용매 3

HCID 66133Benzyl triethylammonium chloride촉매HCID 962Water용매
HCID 6344
Dichloromethane
용매

실험 절차

A solution of sodium hydroxide (16 g) in water (60 ml) was added to a suspension of 3-benzylthio-5-mercapto-1,2,4-triazole (89.2 g) in dichloromethane (400 ml) containing benzyltriethylammonium chloride (1 g) with stirring and cooling to 15°-20° C. To this mixture methyl iodide (56.8 g) was added, and stirring was continued at room temperature for 24 hours. The dichloromethane phase was separated, washed with water twice, dried over magnesium sulphate and run down to give 94 g of crude product, which was recrystallised from toluene to give 80.7 g of desired product, mp 80°-82° C.

후처리

  1. temperaturecooling to 15°-20° C
  2. stirringstirring
  3. customThe dichloromethane phase was separated
  4. washwashed with water twice
  5. dry with materialdried over magnesium sulphate
  6. customto give 94 g of crude product, which
  7. customwas recrystallised from toluene

출처 및 근거

ORD 기록
ord-98b0ffbf77e04d01b7e7b8e3b4d6a01f
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04889553

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