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

Hydrochloric Acid → 1,3,4,5-tetrahydro-1-{1-[(4-methyl-4H,6H-pyrrolo[1,2-a][4,1]benzoxazepin-4-yl)-methyl]-4-piperidinyl}-2H-imidazol-2-one

HRID 845382
노트
인쇄 미리보기

반응식

HRID 845382 반응식
[CH:1]([C:3]1([CH3:17])[O:9][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[CH:15][CH:16]=[C:4]12)=O.Cl.[NH:19]1[CH2:24][CH2:23][CH:22]([N:25]2[CH2:29][CH2:28][NH:27][C:26]2=[O:30])[CH2:21][CH2:20]1.C([BH3-])#N.[Na+]>CO>[CH3:17][C:3]1([CH2:1][N:19]2[CH2:20][CH2:21][CH:22]([N:25]3[CH2:29][CH2:28][NH:27][C:26]3=[O:30])[CH2:23][CH2:24]2)[O:9][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[CH:15][CH:16]=[C:4]12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 5003444Sodium cyanoborohydrideHCID 130317571-(Piperidin-4-yl)imidazolidin-2-oneHCID 141830784-formyl-4-methyl-4H,6H-pyrrolo[1,2-a][4,1]benzoxazepine

생성물 1

HCID 141830791,3,4,5-tetrahydro-1-{1-[(4-methyl-4H,6H-pyrrolo[1,2-a][4,1]benzoxazepin-4-yl)-methyl]-4-piperidinyl}-2H-imidazol-2-one

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 4.5 g of 4-formyl-4-methyl-4H,6H-pyrrolo[1,2-a][4,1]benzoxazepine in 50 ml of methanol is added 3.6 ml of 5.5N methanolic HCl and 3.4 g of 1,3,4,5-tetrahydro-1-(4-piperidinyl)-2H-imidazol-2-one followed by 900 mg of sodium cyanoborohydride. The reaction mixture is allowed to stir at room temperature for 8 days. 2 ml of conc. HCl is added to the reaction mixture and the solvent is removed by evaporation under reduced pressure. The residue is dissolved in 150 ml water and washed with 150 ml of 1:1 ethyl acetate-ether mixture. The aqueous phase is separated, basified with dilute sodium hydroxide to pH 9 and extracted with 2×150 ml of ethyl acetate. The combined ethyl acetate extracts are dried over anhydrous MgSO4, filtered, and the solvent is removed by evaporation under reduced pressure to yield 1,3,4,5-tetrahydro-1-{1-[(4-methyl-4H,6H-pyrrolo[ 1,2-a][4,1]benzoxazepin-4-yl)-methyl]-4-piperidinyl}-2H-imidazol-2-one which is characterized as its maleate salt, m.p. 197°-199°.

후처리

  1. customthe solvent is removed by evaporation under reduced pressure
  2. dissolutionThe residue is dissolved in 150 ml water
  3. washwashed with 150 ml of 1:1 ethyl acetate-ether mixture
  4. customThe aqueous phase is separated
  5. extractionextracted with 2×150 ml of ethyl acetate
  6. dry with materialThe combined ethyl acetate extracts are dried over anhydrous MgSO4
  7. filtrationfiltered
  8. customthe solvent is removed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-75414067f18d4915a0a190e7ac66f456
출처 데이터셋
uspto-grants-1988_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04758559

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트