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Hydrochloric Acid → 4-[[(5,6,7,8-Tetrahydro-5,5-dimethyl-8-oxo-2-naphthalenyl)amino]carbonyl]benzoic acid methyl ester

HRID 53268
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HRID 53268 반응식
[C:1]([O:12][CH3:13])(=[O:11])[C:2]1[CH:10]=[CH:9][C:5]([C:6]([O-:8])=O)=[CH:4][CH:3]=1.[CH3:14][C:15]1([CH3:27])[C:24]2[C:19](=[CH:20][C:21]([NH2:25])=[CH:22][CH:23]=2)[C:18](=[O:26])[CH2:17][CH2:16]1.Cl>S(Cl)(Cl)=O.CN(C)C=O>[CH3:13][O:12][C:1](=[O:11])[C:2]1[CH:3]=[CH:4][C:5]([C:6]([NH:25][C:21]2[CH:22]=[CH:23][C:24]3[C:15]([CH3:14])([CH3:27])[CH2:16][CH2:17][C:18](=[O:26])[C:19]=3[CH:20]=2)=[O:8])=[CH:9][CH:10]=1
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 36144541,4-Benzenedicarboxylic acid, methyl esterHCID 154628417-Amino-4,4-dimethyl-3,4-dihydronaphthalen-1(2H)-one

생성물 1

HCID 537129964-[[(5,6,7,8-Tetrahydro-5,5-dimethyl-8-oxo-2-naphthalenyl)amino]carbonyl]benzoic acid methyl ester

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매
HCID 24386
Thionyl Chloride
용매

실험 절차

A solution of monomethyl terephthalate (VIIIa) (2.86 g, 15.89 mmoles) in thionylchloride (50 mL) with 2 drops of N,N-dimethylformamide was allowed to stir at room temperature. The mixture became homogeneous within 30 minutes and was then concentrated in vacuo. The residue was then taken up in 30 mL of anhydrous pyridine and treated with 4,4-dimethyl-7-amino-1-tetralone (3.00 g, 15.9 mmoles). After 16 hours at room temperature 1N HCl was added to the mixture. It was extracted with ethyl acetate, washed with 1N HCl (4×200 mL) and washed with saturated sodium bicarbonate (2×200 mL). The organic phase was then separated, dried over magnesium sulfate, and concentrated in vacuo to give 5.07 g (Y: 91% ) of the title compound; 1H-NMR (CDCl3): δ8.27 (dd, J=8.7, 2.5 Hz, 1H), 8.19 (bs, 1H), 8.14 (d, J=8.4 Hz, 2H), 7.95 (d, J=8.4 Hz, 2H), 7.91 (d, J=2.5 Hz, 1H), 7.46 (d, J=8.7 Hz, 1H), 3.94 (s, 3H), 2.70 (t, J=7.0 Hz, 3H), 2.00 (t, J=7.0 Hz, 3H), 1.38 (s, 6H); MS (DCI) m/e: 352 (MH+).

후처리

  1. concentrationwas then concentrated in vacuo
  2. extractionIt was extracted with ethyl acetate
  3. washwashed with 1N HCl (4×200 mL)
  4. washwashed with saturated sodium bicarbonate (2×200 mL)
  5. customThe organic phase was then separated
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-493a60e6f8fd4d97a04afa27b4d89495
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05618839

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