홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Carbonate → HCID 22227859, 화합물

HRID 1744577
노트
인쇄 미리보기

반응식

HRID 1744577 반응식
[OH:1][CH2:2][CH2:3][N:4]1[C:8]([CH3:9])=[C:7]([C:10]([OH:12])=O)[CH:6]=[N:5]1.[NH2:13][C:14]1[CH:15]=[CH:16][C:17]([O:22][CH2:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[C:18]([CH:21]=1)[C:19]#[N:20].ON1C2C=CC=CC=2N=N1.C(N=C=NCCCN(C)C)C.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[C:19]([C:18]1[CH:21]=[C:14]([NH:13][C:10]([C:7]2[CH:6]=[N:5][N:4]([CH2:3][CH2:2][OH:1])[C:8]=2[CH3:9])=[O:12])[CH:15]=[CH:16][C:17]=1[O:22][CH2:23][C:24]([CH3:26])([CH3:25])[CH3:27])#[N:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 11430Potassium CarbonateHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 167776201-(2-hydroxyethyl)-5-methyl-1H-pyrazole-4-carboxylic acidHCID 178227345-Amino-2-neopentyloxybenzonitrile

생성물 1

HCID 22227859HCID 22227859, 화합물
수율 30.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-(2-Hydroxyethyl)-5-methylpyrazole-4-carboxylic acid (1.7 g), 5-amino-2-neopentyloxybenzonitrile (2.1 g), 1-hydroxybenzotriazole (1.6 g) and 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide (2.3 g) were added to dimethylformamide (20 ml) and the mixture was stirred at room temperature for 5 h. The reaction mixture was treated with aqueous potassium carbonate solution and extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (mobile phase:chloroform:methanol=100:1). Diisopropyl ether was added to the obtained oily substance to allow crystallization. The crystals were recrystallized from a mixed solvent of ethyl acetate-diisopropyl ether to give the title compound (1.1 g), melting point: 98–100° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customafter which the solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (mobile phase:chloroform:methanol=100:1)
  6. additionDiisopropyl ether was added to the obtained oily substance
  7. customcrystallization
  8. customThe crystals were recrystallized from a mixed solvent of ethyl acetate-diisopropyl ether

출처 및 근거

ORD 기록
ord-93a27f8fd8844ce5bcbd5977e4cf384e
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07015218B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트