Triethylamine → HCID 178429450, 화합물

HRID 577239노트

반응식

HRID 577239 반응식
Br[CH2:2][C:3]1[C:8]([CH3:9])=[CH:7][N:6]=[CH:5][C:4]=1[CH3:10].[CH3:11][C:12]1[N:17]=[C:16]([SH:18])[N:15]=[C:14]([OH:19])[CH:13]=1.C(N(CC)CC)C>C(O)C>[CH3:10][C:4]1[CH:5]=[N:6][CH:7]=[C:8]([CH3:9])[C:3]=1[CH2:2][S:18][C:16]1[N:15]=[C:14]([OH:19])[CH:13]=[C:12]([CH3:11])[N:17]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 595894034-(Bromomethyl)-3,5-dimethylpyridineHCID 178429541HCID 178429541, 화합물

생성물 1

HCID 178429450HCID 178429450, 화합물수율 57%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a 0° C. mixture of 4-(bromomethyl)-3,5-dimethylpyridine (18.6 mmol) and 6-methyl-2-sulfanylpyrimidin-4-ol (1.7 g, 12 mmol) in absolute ethanol (170 mL) was added triethylamine (8 mL, 57.4 mmol). The mixture was stirred at room temperature overnight. The solid precipitate was removed by filtration. Diethyl ether (300 mL) was added to the filtrate. The precipitate was removed by filtration. The filtrate was recovered, evaporated, and co-evaporated with EtOAc (1×50 mL). The residue was treated with water (300 mL). The solid material was recovered by filtration, washed with water (4×30 mL), diethyl ether (3×30 mL) and hexanes (2×30 mL), and dried in vacuo, affording 2-{[(3,5-dimethylpyridin-4-yl)methyl]sulfanyl}-6-methylpyrimidin-4-ol (1.78 g, 57% yield). The product was used without further purification.

후처리

  1. customThe solid precipitate was removed by filtration
  2. additionDiethyl ether (300 mL) was added to the filtrate
  3. customThe precipitate was removed by filtration
  4. customThe filtrate was recovered
  5. customevaporated
  6. additionThe residue was treated with water (300 mL)
  7. filtrationThe solid material was recovered by filtration
  8. washwashed with water (4×30 mL), diethyl ether (3×30 mL) and hexanes (2×30 mL)
  9. customdried in vacuo

출처 및 근거

ORD 기록
ord-86394fe675dd40cd879a17f17dba6dda
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040538B2

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