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

Methanol → (2R,4S)-5-biphenyl-4-yl-4-((2S,3S)-2,3-diacetoxy-3-carboxy-propionylamino)-2-methyl-pentanoic acid

HRID 1469602
노트
인쇄 미리보기

반응식

HRID 1469602 반응식
Cl.C([O:9][C:10](=[O:29])[C@H:11]([CH3:28])[CH2:12][C@H:13]([NH2:27])[CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[CH:17][CH:16]=1)C1C=CC=CC=1.[C:30]([O:33][C@@H:34]1[C:38](=[O:39])[O:37][C:36](=[O:40])[C@H:35]1[O:41][C:42](=[O:44])[CH3:43])(=[O:32])[CH3:31].C(Cl)Cl.N1C=CC=CC=1.CO>C(OCC)(=O)C.[Pd]>[C:18]1([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:17]=[CH:16][C:15]([CH2:14][C@@H:13]([NH:27][C:38](=[O:39])[C@@H:34]([O:33][C:30](=[O:32])[CH3:31])[C@H:35]([O:41][C:42](=[O:44])[CH3:43])[C:36]([OH:37])=[O:40])[CH2:12][C@@H:11]([CH3:28])[C:10]([OH:29])=[O:9])=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 887MethanolHCID 12731855Diacetyltartaric anhydride, D-HCID 21875418Pyridine methylene chlorideHCID 67505899HCID 67505899, 화합물

생성물 1

HCID 49821388(2R,4S)-5-biphenyl-4-yl-4-((2S,3S)-2,3-diacetoxy-3-carboxy-propionylamino)-2-methyl-pentanoic acid

시약·촉매·용매 2

HCID 23938
Palladium
촉매
HCID 8857Ethyl Acetate용매

실험 절차

A solution of (2R,4S)-4-amino-5-biphenyl-4-yl-2-methyl-pentanoic acid benzyl ester hydrochloride (100 mg, 0.287 mmol) and acetic acid (3S,4S)-4-acetoxy-2,5-dioxo-tetrahydro-furan-3-yl ester (0.431 mmol) in 1:1 methylene chloride/pyridine (1.4 mL) is stirred at room temperature for 24 hours. The solvents are removed under reduced pressure and obtained residue is used directly in the subsequent hydrolysis reaction. Next, a solution of the benzyl ester in ethyl acetate is hydrogenated at 1 atm over 10% Pd/C for 18 hours. Methanol is added and the catalyst is filtered through Celite. The Solvent is removed under reduced pressure and the residue is purified by preparative HPLC using a gradient of 10-100% MeCN/water (0.1% TFA). The proper fractions are lyophilized to furnish (2R,4S)-5-biphenyl-4-yl-4-((2S,3S)-2,3-diacetoxy-3-carboxy-propionylamino)-2-methyl-pentanoic acid. HPLC Retention time 0.95 minutes (condition A); MS 500.3 (M+1); 1H NMR (400 MHz, DMSO-d6) δ ppm 1.09 (d, J=7.20Hz, 3H), 1.45 (m, 1H), 1.82 (m, 1H), 2.39 (m, 1H), 2.70 (d, J=6.82Hz, 2H), 4.01 (m, 1H), 5.38 (m, 2H), 7.19 (d, J=8.21Hz, 2H), 7.34 (t, 1H), 7.45 (t, 2H), 7.53 (d, J=8.21Hz, 2H), 7.64 (d, J=7.20Hz, 2H), 8.00 (d, J=8.72Hz, 1H).

후처리

  1. customThe solvents are removed under reduced pressure
  2. customobtained residue
  3. customis used directly in the subsequent hydrolysis reaction
  4. filtrationthe catalyst is filtered through Celite
  5. customThe Solvent is removed under reduced pressure
  6. customthe residue is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-560d5e9d6d9a49c6abcd79be3156b768
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006249B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트