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Hydrochloric Acid → Ethyl[3-(3-{(3,3-diphenylpropyl) [(2e)-3-(4-pyridinyl)-2-propenoyl]amino}propyl)phenoxy]acetate

HRID 2389386
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HRID 2389386 반응식
[N:1]1[CH:6]=[CH:5][C:4](/[CH:7]=[CH:8]/[C:9]([OH:11])=O)=[CH:3][CH:2]=1.C1C=CC2N(O)N=NC=2C=1.[CH2:22]([O:24][C:25](=[O:53])[CH2:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([CH2:34][CH2:35][CH2:36][NH:37][CH2:38][CH2:39][CH:40]([C:47]2[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=2)[C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[CH:29]=1)[CH3:23].Cl>CN(C=O)C.CCOC(C)=O>[CH2:22]([O:24][C:25](=[O:53])[CH2:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([CH2:34][CH2:35][CH2:36][N:37]([CH2:38][CH2:39][CH:40]([C:47]2[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=2)[C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=2)[C:9](=[O:11])/[CH:8]=[CH:7]/[C:4]2[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=2)[CH:29]=1)[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 757711-HydroxybenzotriazoleHCID 7367824-Pyridineacrylic acidHCID 86637891Ethyl (3-{3-[(3,3-diphenylpropyl)amino]propyl}phenoxy)acetate

생성물 1

HCID 59145338Ethyl[3-(3-{(3,3-diphenylpropyl) [(2e)-3-(4-pyridinyl)-2-propenoyl]amino}propyl)phenoxy]acetate

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of (2E)-3-(4-pyridinyl)acrylic acid (23 mg) in DMF (1 mL) was added HOBt (21 mg), ethyl(3-{3-[(3,3-diphenylpropyl)amino]propyl}phenoxy)acetate (55 mg) and WSCD.HCl (29 mg) at ambient temperature. The reaction mixture was stirred for 8 hours at the same temperature. The resulting mixture was diluted with EtOAc and washed successively with water and brine. The organic layer was dried over anhydrous MgSO4, filtered and evaporated in vacuo. The residue was purified by silica gel column chromatography (n-hexane:EtOAc=85:15-70:30) to give a ethyl[3-(3-{(3,3-diphenylpropyl) [(2E)-3-(4-pyridinyl)-2-propenoyl]amino}propyl)phenoxy]acetate.

후처리

  1. customat ambient temperature
  2. washwashed successively with water and brine
  3. dry with materialThe organic layer was dried over anhydrous MgSO4
  4. filtrationfiltered
  5. customevaporated in vacuo
  6. customThe residue was purified by silica gel column chromatography (n-hexane:EtOAc=85:15-70:30)

출처 및 근거

ORD 기록
ord-7e4c7a124d984228927329713844a2ff
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08273745B2

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