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Isobutyl iodide → 2-(4-chlorophenyl)-4-methyl-6-(2-methylpropoxy)-2H-1,2,4-benzothiadiazine-3(4H)-one 1,1-dioxide

HRID 477883
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HRID 477883 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[N:12]([CH3:15])[C:11]3[CH:16]=[C:17]([OH:20])[CH:18]=[CH:19][C:10]=3[S:9]2(=[O:22])=[O:21])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].I[CH2:30][CH:31]([CH3:33])[CH3:32]>C(N)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[N:12]([CH3:15])[C:11]3[CH:16]=[C:17]([O:20][CH2:30][CH:31]([CH3:33])[CH3:32])[CH:18]=[CH:19][C:10]=3[S:9]2(=[O:21])=[O:22])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10556Isobutyl iodideHCID 11430Potassium CarbonateHCID 198724772-(4-chlorophenyl)-6-hydroxy-4-methyl-2H-1,2,4-benzothiadiazine-3(4H)-one 1,1-dioxide

생성물 1

HCID 98436092-(4-chlorophenyl)-4-methyl-6-(2-methylpropoxy)-2H-1,2,4-benzothiadiazine-3(4H)-one 1,1-dioxide수율 58%

시약·촉매·용매 1

HCID 713Formamide
용매

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온도
60 °C

실험 절차

A suspension of 2-(4-chlorophenyl)-6-hydroxy-4-methyl-2H-1,2,4-benzothiadiazine-3(4H)-one 1,1-dioxide (250 mg), potassium carbonate (122 mg) and 1-iodoisobutane (163 mg) in N,Ndimethyl formamide (1 ml) was stirred for 2 hours at 60° C. The mixture was poured into ice water. The separated solid was collected by filtration, dried, and recrystallized from ethanol to yield 2-(4-chlorophenyl)-4-methyl-6-(2-methylpropoxy)-2H-1,2,4-benzothiadiazine-3(4H)-one 1,1-dioxide (169 mg).

후처리

  1. filtrationThe separated solid was collected by filtration
  2. customdried
  3. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-ebd64f967cde4772ba2d701b359d0b01
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04889851

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