Sodium Chloride → tert-Butyl 2-(3,4-dichloro-N-methylphenylsulfonamido)-4,5,6,7-tetrahydrobenzo-[b]thiophene-3-carboxylate

HRID 1642125노트

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HRID 1642125 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([NH:12][C:13]2[S:17][C:16]3[CH2:18][CH2:19][CH2:20][CH2:21][C:15]=3[C:14]=2[C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].[C:29]([O-])([O-])=O.[K+].[K+].CI.[Na+].[Cl-]>CC(C)=O.O>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:12]([C:13]2[S:17][C:16]3[CH2:18][CH2:19][CH2:20][CH2:21][C:15]=3[C:14]=2[C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH3:29])(=[O:10])=[O:11])[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

7

반응물 4

HCID 5234Sodium ChlorideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86625455tert-Butyl 2-(3,4-dichlorophenylsulfonamido)-4,5,6,7-tetrahydrobenzo[b]-thiophene-3-carboxylate

생성물 1

HCID 66756439tert-Butyl 2-(3,4-dichloro-N-methylphenylsulfonamido)-4,5,6,7-tetrahydrobenzo-[b]thiophene-3-carboxylate

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

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온도
40 °C

실험 절차

tert-Butyl 2-(3,4-dichlorophenylsulfonamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate (21.64 g, 46.8 mmol) was dissolved in acetone (200 ml), and K2CO3 (12.9 g, 93.6 mmol) was added thereto. Methyl iodide (5.83 ml, 93.6 mmol) was then added, and the suspension was heated overnight at 40° C. After cooling to room temperature, water and saturated NaCl solution were added and the product was extracted with ethyl acetate. The organic phase was dried (sodium sulfate) and the product was purified by crystallization from methanol.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionthe product was extracted with ethyl acetate
  3. dry with materialThe organic phase was dried (sodium sulfate)
  4. customthe product was purified by crystallization from methanol

출처 및 근거

ORD 기록
ord-9ad16240addf439ea3b53b7601ff98fa
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119633B2

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