Diethyl Malonate → HCID 178516644, 화합물

HRID 530737노트

반응식

HRID 530737 반응식
CC[O-].[Na+].Cl.[F:6][C:7]([F:17])([F:16])[C:8]1[N:9]=[C:10]([C:13]([NH2:15])=[NH:14])[S:11][CH:12]=1.[C:18](OCC)(=[O:25])[CH2:19][C:20](OCC)=[O:21]>CCO>[F:17][C:7]([F:6])([F:16])[C:8]1[N:9]=[C:10]([C:13]2[N:15]=[C:20]([OH:21])[CH:19]=[C:18]([OH:25])[N:14]=2)[S:11][CH:12]=1

참가 물질

5

반응물 3

HCID 7761Diethyl MalonateHCID 2723922Sodium ethoxideHCID 667304744-(Trifluoromethyl)thiazole-2-carboximidamide hydrochloride

생성물 1

HCID 178516644HCID 178516644, 화합물수율 98%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred solution of NaOEt (32 g, 5 eq.) in EtOH (200 mL) was slowly added compound 282 (22 g, 1 eq.). The reaction mixture was stirred at room temperature for 30 min and diethyl malonate (11.5 mL, 0.8 eq.) was then added. The suspension was refluxed for 24 hrs. The solvent was removed under reduced pressure. The residue was suspended in H2O (200 mL) and acidified to pH 5 with 2 N aqueous HCl. The resulting solid was filtered, washed with water, and dried under reduced pressure to yield compound 283 as a brown solid in 98% yield. 1H NMR (DMSO-d6, 400 MHz) δ 5.77 (s, 1H), 8.68 (s, 1H).

후처리

  1. temperatureThe suspension was refluxed for 24 hrs
  2. customThe solvent was removed under reduced pressure
  3. filtrationThe resulting solid was filtered
  4. washwashed with water
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-8a3c7c5829324d51a0c5bd235c1aa426
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353100B2

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