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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethyl 2-(diphenylmethyleneamino)acetate → (S)-2-(benzhydrylidene-amino)-4-methyl-hexanoic acid ethyl ester

HRID 19405
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HRID 19405 반응식
[CH2:1]([O:3][C:4](=[O:20])[CH2:5][N:6]=[C:7]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH3:2].CC(C)([O-])C.[K+].I[CH2:28][C@@H:29]([CH3:32])[CH2:30][CH3:31]>O1CCCC1>[CH2:1]([O:3][C:4](=[O:20])[C@@H:5]([N:6]=[C:7]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[CH2:28][CH:29]([CH3:32])[CH2:30][CH3:31])[CH3:2]
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참가 물질

5

반응물 3

HCID 319508Ethyl 2-(diphenylmethyleneamino)acetateHCID 5702528(S)-(+)-1-Iodo-2-methylbutaneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 86635244(S)-2-(benzhydrylidene-amino)-4-methyl-hexanoic acid ethyl ester수율 74%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

A solution of (benzhydrylidene-amino)-acetic acid ethyl ester (5.48 g, 20.5 mmol) in tetrahydrofuran (40 mL) was treated with potassium t-butoxide (2.83 g, 25.26 mmol) and stirred at 0° C. for 35 min. At this time a solution of (S)-1-iodo-2-methyl-butane (5.00 g, 25.25 mmol) in tetrahydrofuran (20 mL) was added via syringe and the resulting solution stirred at 0° C. for 10 min and then room temperature overnight. The reaction mixture was concentrated in vacuo and the residue partitioned between diethyl ether and dilute aqueous hydrochloric acid. The layers were separated, and the organic layer was washed with brine and concentrated in vacuo. The residue was purified by ISCO flash chromatography (RediSep silica 120 g, 0% to 10% ethyl acetate/hexanes) which afforded (S)-2-(benzhydrylidene-amino)-4-methyl-hexanoic acid ethyl ester (5.09 g, 74%) as an oil.

후처리

  1. stirringthe resulting solution stirred at 0° C. for 10 min
  2. customroom temperature overnight
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. customthe residue partitioned between diethyl ether and dilute aqueous hydrochloric acid
  5. customThe layers were separated
  6. washthe organic layer was washed with brine
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by ISCO flash chromatography (RediSep silica 120 g, 0% to 10% ethyl acetate/hexanes) which

출처 및 근거

ORD 기록
ord-e2b1e4a3f0e64d58bf4a398c4d0d1a9d
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07741327B2

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