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Dichloroisoproterenol → (4-{3-[2-(3,4-Dichloro-phenyl)-2-hydroxy-ethyl]-3-isopropyl-ureido}-benzyl)-carbamic acid tert-butyl ester

HRID 1057977
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HRID 1057977 반응식
ClC(Cl)([O:4][C:5](=O)[O:6]C(Cl)(Cl)Cl)Cl.[NH2:13][C:14]1[CH:21]=[CH:20][C:17]([CH2:18][NH2:19])=[CH:16][CH:15]=1.[C:22]([NH:26][C:27](=[O:29])[O-])([CH3:25])([CH3:24])C.C(N([CH:36]([CH3:38])[CH3:37])CC)(C)C.C(N[CH2:43][CH:44]([C:46]1[CH:51]=[CH:50][C:49]([Cl:52])=[C:48]([Cl:53])[CH:47]=1)[OH:45])(C)C.[CH2:54](Cl)Cl>CCOC(C)=O>[C:36]([O:6][C:5](=[O:4])[NH:19][CH2:18][C:17]1[CH:20]=[CH:21][C:14]([NH:13][C:27]([N:26]([CH2:43][CH:44]([C:46]2[CH:51]=[CH:50][C:49]([Cl:52])=[C:48]([Cl:53])[CH:47]=2)[OH:45])[CH:22]([CH3:24])[CH3:25])=[O:29])=[CH:15][CH:16]=1)([CH3:38])([CH3:54])[CH3:37]
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참가 물질

8

반응물 6

HCID 5806DichloroisoproterenolHCID 6344Dichloromethane3회HCID 81531Diisopropylethylamine2회HCID 94429TriphosgeneHCID 4278144-AminobenzylamineHCID 21252905Tert-butylcarbamate

생성물 1

HCID 23560247
(4-{3-[2-(3,4-Dichloro-phenyl)-2-hydroxy-ethyl]-3-isopropyl-ureido}-benzyl)-carbamic acid tert-butyl ester

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 0.89 g (3 mmol) triphosgene in 10 ml CH2Cl2 was added a solution of 2.0 g (8 mmol) 4-aminobenzylamine, tertbutylcarbamate and 1.69 ml (9.7 mmol) diisopropylethylamine in 25 ml CH2Cl2 dropwise over 1 hour. After the addition was complete, a solution of 1.79 g (8 mmol) 2-isopropylamino-1-(3,4-dichlorophenyl)-ethanol and 1.69 ml (9.7 mmol) diisopropylethylamine in 25 ml CH2Cl2 was added over 5 min. The reaction mixture was stirred for 10 min. diluted with 200 ml EtOAc, washed with 200 ml each of saturated aqueous NaHCO3, water, and brine, then dried over Na2SO4 , filtered and concentrated. Purification by flash chromatography (50% EtOAc/hexanes) provided 4 g (4-{3-[2-(3,4-Dichloro-phenyl)-2-hydroxy-ethyl]-3-isopropyl-ureido}-benzyl)-carbamic acid tert-butyl ester. 1H NMR (300 mHz, CDCl3) 8.85 (br s, 1H); 7.45 (m, 2H); 7.3-7.0 (m, 5H); 5.82 (s, 1H); 5.12 (br s, 1H); 4.7 (d, 1H, J=8 Hz); 4.4-4.15 (m, 3H); 3.42 (dd, 1H, J=16 and 8 Hz); 3.1 (d, 1H, J=16 Hz); 1.4 (s, 9H); 1.9 (d, 3H, J=7 Hz); 1.07 (d, 3H, J=7 Hz).

후처리

  1. additionAfter the addition
  2. washwashed with 200 ml each of saturated aqueous NaHCO3, water, and brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by flash chromatography (50% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-e1d3fd509dbc4835ae3bc74edbf4c248
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06515023B2

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