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

Ethyl Acetate → 3-Ethyl-2,3,9,10,11,12-hexahydro-1-methyl-1H-quino[4,3,2-ef][1,4]benzoxazepine fumarate

HRID 981940
노트
인쇄 미리보기

반응식

HRID 981940 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-].[CH2:11]([CH:13]1[C:19](=[O:20])[N:18]([CH3:21])[C:17]2=[C:22]3[C:27](=[N:28][C:29]4=[CH:30][CH:31]=[CH:32][C:15](=[C:16]24)[O:14]1)[CH2:26][CH2:25][CH2:24][CH2:23]3)[CH3:12].[OH-:33].[Na+].[C:35]([O:38]CC)(=[O:37])[CH3:36]>O1CCCC1>[C:19]([OH:20])(=[O:33])/[CH:13]=[CH:36]/[C:35]([OH:38])=[O:37].[CH2:11]([CH:13]1[CH2:19][N:18]([CH3:21])[C:17]2=[C:22]3[C:27](=[N:28][C:29]4=[CH:30][CH:31]=[CH:32][C:15](=[C:16]24)[O:14]1)[CH2:26][CH2:25][CH2:24][CH2:23]3)[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 21226445Aluminium lithium hydrideHCID 538029823-ethyl-1,3,9,10,11,12-hexahydro-1-methyl-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one

생성물 1

HCID 67756603
3-Ethyl-2,3,9,10,11,12-hexahydro-1-methyl-1H-quino[4,3,2-ef][1,4]benzoxazepine fumarate
수율 38%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of lithium aluminum hydride in tetrahydrofuran (1M, 11.99 ml) and dry tetrahydrofuran (30 ml) was added aluminum chloride (1.6 g) in portions, with stirring. After five mins, 3-ethyl-1,3,9,10,11,12-hexahydro-1-methyl-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one (3.55 g) was added, and stirring was continued for 0.5 hr. Ethyl acetate (200 ml) and 10% sodium hydroxide solution (200 ml) were added, the organic layer was separated, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated. The residue was flash chromatographed (1.5% triethylamine/toluene). The appropriate fractions were concentrated and the residue was treated with fumaric acid followed by recrystallization from methanol to give 1.82 g (38%) of product, mp 243° C. (dec.).

후처리

  1. stirringstirring
  2. waitwas continued for 0.5 hr
  3. customthe organic layer was separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated
  7. customchromatographed (1.5% triethylamine/toluene)
  8. concentrationThe appropriate fractions were concentrated
  9. additionthe residue was treated with fumaric acid
  10. customfollowed by recrystallization from methanol

출처 및 근거

ORD 기록
ord-76e287b6f2c34491a4397ed20cb2334f
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04994452

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트