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

Sodium Carbonate → HCID 59065920, 화합물

HRID 25743
노트
인쇄 미리보기

반응식

HRID 25743 반응식
[Si:1]([O:8][C@H:9]1[C@@H:13]([O:14][Si:15]([C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:17])[CH3:16])[C@H:12]([N:22]2[CH:27]=[CH:26][C:25](=[O:28])[NH:24][C:23]2=[O:29])[O:11][CH:10]1[C@H:30]([OH:62])[C@@H:31]([C:55]([O:57][C:58]([CH3:61])([CH3:60])[CH3:59])=[O:56])[NH:32][CH2:33][CH2:34][CH2:35][NH:36][C:37](=[O:54])[C@H:38]([CH2:50][CH:51]([CH3:53])[CH3:52])[NH:39][C:40](=[O:49])[O:41][CH2:42][C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[CH2:63](OC(=O)N[C@@H](C(=O)NCCC=O)CC(C)C)[C:64]1[CH:69]=[CH:68][CH:67]=[CH:66][CH:65]=1.[C:86](N[C@@H](C(O)=O)CC(C)C)(OCC1C=CC=CC=1)=[O:87].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1.C(O)(=O)C>[Si:1]([O:8][C@H:9]1[C@@H:13]([O:14][Si:15]([C:18]([CH3:19])([CH3:21])[CH3:20])([CH3:17])[CH3:16])[C@H:12]([N:22]2[CH:27]=[CH:26][C:25](=[O:28])[N:24]([CH2:63][C:64]3[CH:65]=[CH:66][C:67]([O:87][CH3:86])=[CH:68][CH:69]=3)[C:23]2=[O:29])[O:11][CH:10]1[C@H:30]([OH:62])[C@@H:31]([C:55]([O:57][C:58]([CH3:60])([CH3:59])[CH3:61])=[O:56])[NH:32][CH2:33][CH2:34][CH2:35][NH:36][C:37](=[O:54])[C@@H:38]([CH2:50][CH:51]([CH3:52])[CH3:53])[NH:39][C:40](=[O:49])[O:41][CH2:42][C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)([C:4]([CH3:5])([CH3:6])[CH3:7])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 10340Sodium CarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 7000099N-Cbz-D-leucineHCID 59065937HCID 59065937, 화합물HCID 86587959[(1R)-3-methyl-1-(3-oxo-propylcarbamoyl)butyl]-carbamic acid benzyl ester

생성물 1

HCID 59065920
HCID 59065920, 화합물
수율 42%

시약·촉매·용매 2

HCID 176Acetic Acid촉매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of tert-butyl (5S,12S)-12-[(R)-[(3R,4R,5R)-3,4-bis{[tert-butyl(dimethyl)silyl]oxy}-5-(2,4-dioxo-3,4-dihydro-1(2H)-pyrimidinyl)tetrahydro-2-furanyl](hydroxy)methyl]-5-isobutyl-3,6-dioxo-1-phenyl-2-oxa-4,7,11-triazatridecan-13-oate (62 mg, 0.086 mmol, obtained from Reference Example 6) and [(1R)-3-methyl-1-(3-oxo-propylcarbamoyl)butyl]-carbamic acid benzyl ester (33 mg, 0.103 mmol, obtained from N-CBZ-D-leucine in an similar manner described in Reference Example 15 and 16) in anhydrous tetrahydrofuran was stirred at room temperature under a nitrogen atmosphere for 15 minutes. Acetic acid (2 drops) and sodium triacetoxyborohydride (36 mg, 0.17 mmol) were added and the resulting solution was stirred under nitrogen for an additional 2.5 hours. The reaction mixture was basified to pH 9 with aqueous sodium carbonate solution and the aqueous layer was extracted with ethyl acetate (3×50 ml). The combined extracts were washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated in vacuo. The residue was chromatographed (flash column, silica gel, 2.5% methanol in methylene chloride) to provide tert-butyl (5R,12S)-12-[(R)-[(3R,4R,5R)-3,4-bis{[tert-butyl(dimethyl)silyl]oxy}-5-(3-(4-methoxybenzyl)-2,4-dioxo-3,4-dihydro-1(2H)-pyrimidinyl)tetrahydro-2-furanyl](hydroxy)methyl]-5-isobutyl-3,6-dioxo-1-phenyl-2-oxa-4,7,11-triazatridecan-13-oate (37 mg, 42%) as a white amorphous solid.

후처리

  1. stirringthe resulting solution was stirred under nitrogen for an additional 2.5 hours
  2. extractionthe aqueous layer was extracted with ethyl acetate (3×50 ml)
  3. washThe combined extracts were washed with saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was chromatographed (flash column, silica gel, 2.5% methanol in methylene chloride)

출처 및 근거

ORD 기록
ord-63c2ee21c7524ffc9ef2d2ecedbbf78a
출처 데이터셋
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06858591B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트