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

1,2-Cyclohexanedione → HCID 178439981, 화합물

HRID 1904340
노트
인쇄 미리보기

반응식

HRID 1904340 반응식
[C:1]1(=O)[CH2:6][CH2:5][CH2:4][CH2:3][C:2]1=O.Cl.[NH2:10][C@H:11]([C:15]([NH2:17])=[O:16])[CH2:12][CH2:13][CH3:14].[OH-].[Na+]>CO>[OH:16][C:15]1[C:11]([CH2:12][CH2:13][CH3:14])=[N:10][C:1]2[CH2:6][CH2:5][CH2:4][CH2:3][C:2]=2[N:17]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 130061,2-CyclohexanedioneHCID 14798Sodium HydroxideHCID 56777018(2S)-2-aminopentanamide hydrochloride

생성물 1

HCID 178439981HCID 178439981, 화합물수율 50%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
-30 °C

실험 절차

1,2-cyclohexanedione (5.4 g, 48 mM) was added all at once to a methanol solution (80 ml) of norvalineamide hydrochloride (6.1 g, 40 mM) at -30° C., and aqueous 12.5N NaOH (8 ml) was added dropwise thereto. The reaction mixture was stirred at -30° C. for 30 mins., cooling was removed, and the mixture stirred to room temperature for 3 hours. Conc. hydrochloric aicd (10 ml) was added to the reaction mixture under ice-cooling, sodium bicarbonate (8 g) was added after 10 mins., the methanol then being distilled off in vacuo. The residue was extracted with chloroform, and the extract washed with water, dried with anhydrous sodium sulfate and concentrated in vacuo. The residue was washed with acetone and recrystallized from acetone to obtain the product as colorless crystals (3.8 g., yield: 50%, m.p.: 131°-133° C.).

후처리

  1. temperature, cooling
  2. customwas removed
  3. stirringthe mixture stirred to room temperature for 3 hours
  4. additionConc. hydrochloric aicd (10 ml) was added to the reaction mixture under ice-
  5. temperaturecooling
  6. additionsodium bicarbonate (8 g) was added after 10 mins
  7. distillation, the methanol then being distilled off in vacuo
  8. extractionThe residue was extracted with chloroform
  9. washthe extract washed with water
  10. dry with materialdried with anhydrous sodium sulfate
  11. concentrationconcentrated in vacuo
  12. washThe residue was washed with acetone
  13. customrecrystallized from acetone

출처 및 근거

ORD 기록
ord-5b3bb45e78634643b02b062947e1cf40
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04837319

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트