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

Ammonium Chloride → HCID 44596871, 화합물

HRID 553556
노트
인쇄 미리보기

반응식

HRID 553556 반응식
[C:1]([N:9]1[C@H:13]([CH3:14])[C:12](=[O:15])[O:11][C@H:10]1[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C.[CH3:32][O:33][C:34]1[CH:41]=[CH:40][C:37]([CH2:38]Br)=[CH:36][CH:35]=1.[NH4+].[Cl-]>C1COCC1>[CH3:32][O:33][C:34]1[CH:41]=[CH:40][C:37]([CH2:38][C@:13]2([CH3:14])[C:12](=[O:15])[O:11][C@@H:10]([C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=3)[N:9]2[C:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[O:8])=[CH:36][CH:35]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 1650214-Methoxybenzyl bromideHCID 2733832Lithium hexamethyldisilazaneHCID 13818180(2S,4R)-3-Benzoyl-4-methyl-2-phenyl-1,3-oxazolidin-5-one

생성물 1

HCID 44596871HCID 44596871, 화합물수율 82%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

반응 조건

온도
-78 °C

실험 절차

Compound 2.2 (6.35 g, 0.023 mol) in 50 mL of THF at −78° C. was added over 20 min to a solution of LHMDS in THF (25 mL of 1 M solution in THF). After 10 min, 1.1 eq. of 4-methoxybenzyl bromide (25 mmol, 5 mL) was added in one portion. The mixture was stirred at −78° C. for 3 h and then room temperature overnight. Saturated NH4Cl solution was added, the THF was removed in vacuo, 100 mL of Et2O was added and the phases were separated. The organic layer was washed with 50 mL of NaHCO3 solution and brine. After drying (Na2SO4), filtration and removal of the solvent, the residue was purified by chromatography using Si Gel ISCO column with 9% EtOAc in Hexanes as eluent. Concentration of the product fractions gave 7.4 g (82%) of 2.3 as a white solid. MP 128-129° C.; [α]25D=−260 (c 0.8, MeOH); 1H NMR δ 7.27 (1H, d, J=8 Hz), 7.19-7.14 (2H, m), 7.09-7.05 (4H, m), 6.94 (d, 2H, J=8 Hz), 6.76-6.72 (m, 4H), 5.68 (s, 1H), 3.88 (d, 1H, J=12 Hz), 3.86 (s, 3H), 3.27 (d, 1H, J=12 Hz), 2.14 (s, 3H); C NMR 175.1, 169.4, 159.6, 136.7, 131.5, 130.1, 130.0, 128.8, 128.7, 128.2, 127.2, 126.3, 114.6, 90.7, 65.9, 55.8, 40.5, 24.6; ESI MS 402 (M+1).

후처리

  1. customroom temperature overnight
  2. customthe THF was removed in vacuo, 100 mL of Et2O
  3. additionwas added
  4. customthe phases were separated
  5. washThe organic layer was washed with 50 mL of NaHCO3 solution and brine
  6. customAfter drying
  7. filtration(Na2SO4), filtration and removal of the solvent
  8. customthe residue was purified by chromatography

출처 및 근거

ORD 기록
ord-b3832f035a014ba69c903abd40c6799e
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08048895B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트