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Triethylamine → hexane ethyl acetate 6-chloro-2-(4-bromobutyl)-2H-thieno[3,2-e]-1,2-thiazine 1,1-dioxide

HRID 1061492
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HRID 1061492 반응식
[Cl:1][C:2]1[S:10][C:9]2[S:8](=[O:12])(=[O:11])[N:7]([CH2:13][CH2:14][CH2:15][CH2:16][Br:17])[CH2:6][CH:5]([OH:18])[C:4]=2[CH:3]=1.[CH2:19](N([CH2:24][CH3:25])CC)C.CS(OS(C)(=O)=O)(=O)=[O:28]>O1CCCC1>[CH3:19][CH2:6][CH2:5][CH2:4][CH2:3][CH3:2].[Cl:1][C:2]1[S:10][C:9]2[S:8](=[O:12])(=[O:11])[N:7]([CH2:13][CH2:14][CH2:15][CH2:16][Br:17])[CH:6]=[CH:5][C:4]=2[CH:3]=1.[C:24]([O:18][CH2:5][CH3:6])(=[O:28])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 81560Methanesulfonic anhydrideHCID 220580556-chloro-3,4-dihydro-2-(4-bromobutyl)-2H-thieno[3,2-e]-1,2-thiazine-4-ol 1,1-dioxide

생성물 1

HCID 86600312hexane ethyl acetate 6-chloro-2-(4-bromobutyl)-2H-thieno[3,2-e]-1,2-thiazine 1,1-dioxide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The product from Step 1 (10.6 g, 28.3 mmol) was dissolved in tetrahydrofuran (anhydrous, 400 mL) and treated with triethyl amine (9.88 mL, 70.9 mmol) and methane sulfonic anhydride (9.86 g, 56.6 mmol) at room temperature and stirred for one hour. The suspension was concentrated and taken up in dimethylformamide (anhydrous, 120 mL). This mixture was heated at 160° for 45 min. The reaction mixture was poured into ice water (300 ml) and extracted with dichloromethane (300 mL). The organic layer was washed with water (2×200 mL), dried over magnesium sulfate and evaporated to a brown oil. After silica flash chromatography with hexane/ethyl acetate 6-chloro-2-(4-bromobutyl)-2H-thieno[3,2-e]-1,2-thiazine 1,1-dioxide was obtained as a yellow oil (4.97 g, 49%); the 1H NMR. was consistent with the structure.

후처리

  1. concentrationThe suspension was concentrated
  2. temperatureThis mixture was heated at 160° for 45 min
  3. additionThe reaction mixture was poured into ice water (300 ml)
  4. extractionextracted with dichloromethane (300 mL)
  5. washThe organic layer was washed with water (2×200 mL)
  6. dry with materialdried over magnesium sulfate
  7. customevaporated to a brown oil

출처 및 근거

ORD 기록
ord-1e7915a5ae9f44cb94d83ace0d529126
출처 데이터셋
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06960579B1

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