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Potassium thiocyanate → (S)-2-(2-amino-7-bromo-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyethyl pivalate

HRID 879273
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HRID 879273 반응식
[C:1]([O:7][CH2:8][C@H:9]([C:15]1[C:20]([CH3:21])=[CH:19][C:18]([NH2:22])=[CH:17][C:16]=1[Br:23])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].[C:24]([S-:26])#[N:25].[K+].[NH+]1C=CC=CC=1.C([O-])(O)=O.[Na+]>CC(O)=O>[C:1]([O:7][CH2:8][C@H:9]([C:15]1[C:20]([CH3:21])=[CH:19][C:18]2[N:22]=[C:24]([NH2:25])[S:26][C:17]=2[C:16]=1[Br:23])[O:10][C:11]([CH3:12])([CH3:13])[CH3:14])(=[O:6])[C:2]([CH3:3])([CH3:4])[CH3:5]
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참가 물질

6

반응물 4

HCID 516872Potassium thiocyanateHCID 516892Sodium BicarbonateHCID 4989215PyridiniumHCID 86699788(S)-2-(4-amino-2-bromo-6-methylphenyl)-2-tert-butoxyethyl pivalate

생성물 1

HCID 86699789(S)-2-(2-amino-7-bromo-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyethyl pivalate수율 34.3%

시약·촉매·용매 1

HCID 176
Acetic Acid
용매

실험 절차

To a solution of freshly prepared (S)-2-(4-amino-2-bromo-6-methylphenyl)-2-tert-butoxyethyl pivalate (7 g, 18.1 mmol) in HOAc (90 mL) was added KSCN (1.76 g, 18.1 mmol) at r.t. The reaction mixture was stirred at r.t. for 0.5 h. Pyridinium perbromide (5.79 g, 18.1 mmol) was added slowly over a period of 10 min, and stirred at r.t for 2 h. The mixture was alkalized to pH=8 using saturated aqueous NaHCO3 solution, then extracted with EtOAc (3×600 mL). The combined organic layers were dried over anhydrous Na2SO4, filtered, concentrated in vacuo, and purified by silica gel column (Petroleum Ether:EtOAc (10:1→5:1)) to afford (S)-2-(2-amino-7-bromo-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyethyl pivalate (2.74 g, 34.3%) as yellow solid. LCMS-ESI+: calc'd for C19H27BrN2O3S: 443.1 and 445.1 (M+H+); found: 443.1 and 445.1 (M+H+). 1H-NMR: 400 MHz, (CD3OD) δ: 7.15 (s, 1H), 5.53-5.49 (m, 1H), 4.31-4.26 (m, 1H), 4.17-4.13 (m, 1H), 2.64 (s, 3H), 1.15 (s, 9H), 1.11 (s, 9H).

후처리

  1. stirringstirred at r.t for 2 h
  2. extractionextracted with EtOAc (3×600 mL)
  3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. custompurified by silica gel column (Petroleum Ether:EtOAc (10:1→5:1))

출처 및 근거

ORD 기록
ord-809ed9e1a4eb46d38eb4eed124720cf3
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987250B2

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