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

Iodoethane → 7-Chloro-3-ethyl-1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one

HRID 580385
노트
인쇄 미리보기

반응식

HRID 580385 반응식
[CH:1]([N-]C(C)C)(C)[CH3:2].[Li+].C([Li])CCC.C(NC(C)C)(C)C.[Cl:21][C:22]1[CH:23]=[CH:24][C:25]2[NH:31][C:30](=[O:32])[CH:29]([C:33]([O:35][CH3:36])=[O:34])[CH:28]([C:37]3[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[CH:39][CH:38]=3)[CH2:27][C:26]=2[CH:45]=1.ICC.C(=O)=O.C(Cl)(Cl)(Cl)Cl>O1CCCC1.CCCCCC.CN(C)P(=O)(N(C)C)N(C)C>[Cl:21][C:22]1[CH:23]=[CH:24][C:25]2[NH:31][C:30](=[O:32])[C:29]([CH2:1][CH3:2])([C:33]([O:35][CH3:36])=[O:34])[CH:28]([C:37]3[CH:38]=[CH:39][C:40]([O:43][CH3:44])=[CH:41][CH:42]=3)[CH2:27][C:26]=2[CH:45]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 6

HCID 6340IodoethaneHCID 7912DiisopropylamineHCID 2724682Lithium diisopropylamideHCID 141561947-Chloro-1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-oneHCID 86602444Carbontetrachloride dry-iceHCID 178418339Butyllithium

생성물 1

HCID 15128680
7-Chloro-3-ethyl-1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one

시약·촉매·용매 3

HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매HCID 12679Hexamethylphosphoramide용매

반응 조건

온도
-78 °C

실험 절차

To a freshly prepared solution of lithium diisopropylamide in tetrahydrofuran (6 equivalents; prepared by addition of 19.2 ml of a 2.6M solution of n-butyllithium in hexane to 15 ml of freshly distilled diisopropylamine in 80 ml of tetrahydrofuran) at -78° C., was added 3.0 g (8.35 mmole) of 7-chloro-1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one (see Example 1C . After stirring at -78° C. for 1.5 hours, 3 ml of hexamethylphosphoric triamide was added along with 13.6 ml of iodoethane (filtered through alumina to remove iodine). The mixture was stirred at -78° C. for 30 minutes (under argon), and then at -20° C. (dry-ice/carbon tetrachloride bath) for six days. The reaction was quenched with 1N hydrochloric acid (50 ml), and the aqueous layer was extracted with ethyl acetate (three times). The ethyl acetate extracts and the tetrahydrofuran were combined, washed with saturated sodium bicarbonate and saturated sodium chloride, and dried (magnesium sulfate). The solution was concentrated, combined with 0.31 g of previously prepared crude product and flash chromatographed (silica gel/3:1-hexane:ethyl acetate) yielding 0.61 g of product.

후처리

  1. stirringThe mixture was stirred at -78° C. for 30 minutes (under argon)
  2. customThe reaction was quenched with 1N hydrochloric acid (50 ml)
  3. extractionthe aqueous layer was extracted with ethyl acetate (three times)
  4. washwashed with saturated sodium bicarbonate and saturated sodium chloride
  5. dry with materialdried (magnesium sulfate)
  6. concentrationThe solution was concentrated
  7. customof previously prepared crude product and flash
  8. customchromatographed (silica gel/3:1-hexane:ethyl acetate)

출처 및 근거

ORD 기록
ord-ef2f98eaa704433298f15a3ed1736cee
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04752645

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트