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Hydrochloric Acid → HCID 67243180, 화합물

HRID 729243
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HRID 729243 반응식
CC(C)([O-])C.[K+].[C:7]([NH:11][S:12]([CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:14])=[O:13])([CH3:10])([CH3:9])[CH3:8].[C:22](OCC)(=[O:28])[C:23](OCC)=[O:24].Cl>C1COCC1>[C:7]([N:11]1[C:23](=[O:24])[C:22]([OH:28])=[C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[S:12]1(=[O:14])=[O:13])([CH3:10])([CH3:8])[CH3:9]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 562762N-tert-butyl-1-phenylmethanesulfonamideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 67243180HCID 67243180, 화합물수율 471.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
150 °C

실험 절차

Potassium tert-butoxide (0.845 g, 10.56 mmol) was added to a solution of N-(tert-butyl)-1-phenylmethanesulfonamide (1.2 g, 5.28 mmol) and diethyl oxalate (0.85 mL, 6.33 mmol) in THF (8 mL) and the mixture was heated at 150° C. for 15 mins in a microwave reactor. The reaction mixture was acidified with 1M HCl, the THF was evaporated and the residue was extracted with DCM. The mixture was evaporated, the residue was triturated in petroleum ether and the solvent was decanted to give the title compound (7 g, 63%) as a solid; 1H NMR (500 MHz, CDCl3): δ 7.44-7.32 (m, 5H), 3.90 (br s, 1H), 1.36 (s, 9H); Mass Spectrum: M−H+280

후처리

  1. customthe THF was evaporated
  2. extractionthe residue was extracted with DCM
  3. customThe mixture was evaporated
  4. customthe residue was triturated in petroleum ether
  5. customthe solvent was decanted

출처 및 근거

ORD 기록
ord-c567e8fa42ad4663ad7a0baaf04387ee
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582629B2

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