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

N-(Diphenylmethylene)glycine tert-butyl ester → 2-(Benzhydrylidene-amino)-3-cycloheptyl-propionic acid tert-butyl ester

HRID 1018846
노트
인쇄 미리보기

반응식

HRID 1018846 반응식
[C:1]([O:5][C:6](=[O:22])[CH2:7][N:8]=[C:9]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([CH3:4])([CH3:3])[CH3:2].C([N-]C(C)C)(C)C.[Li+].[CH:31]1([CH2:38]I)[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1>O1CCCC1>[C:1]([O:5][C:6](=[O:22])[CH:7]([N:8]=[C:9]([C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)[CH2:38][CH:31]1[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 688171N-(Diphenylmethylene)glycine tert-butyl esterHCID 2724682Lithium diisopropylamideHCID 2763013Iodomethylcycloheptane

생성물 1

HCID 865853992-(Benzhydrylidene-amino)-3-cycloheptyl-propionic acid tert-butyl ester수율 73%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a stirred solution of (Benzhydrylidene-amino)-acetic acid tert-butyl ester (2.56 g; 8.68 mmol) in 30 mL of tetrahydrofuran under argon at −78° C. was added lithium diisopropylamide solution (10.0 mL; 1.5 M solution in cyclohexane) dropwise. After 30 minutes, a solution of cycloheptylmethyl iodide (Prepared in Step B; 3.48 g; 14.6 mmol) in 20 mL tetrahydrofuran was added dropwise and the mixture allowed to warm to room temperature and stirred for 18 h. The mixture was quenched with saturated ammonium chloride solution (100 mL). The layers were separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were dried (sodium sulfate) filtered and concentrated in vacuo. The crude product was chromatographed (Biotage 40M; eluent: 5% ethyl acetate/hexanes) to give 2.56 g (73%) of 2-(Benzhydrylidene-amino)-3-cycloheptyl-propionic acid tert-butyl ester as a pale yellow oil.

후처리

  1. customThe mixture was quenched with saturated ammonium chloride solution (100 mL)
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with ethyl acetate
  4. dry with materialThe combined organic layers were dried (sodium sulfate)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude product was chromatographed (Biotage 40M; eluent: 5% ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-1acd85e0fa9e4ad897b3a0cf47553bc7
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06482951B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트