Ethyl Acetate → 2-{[(Benzyloxy)carbonyl]amino}-3-(3-{[(t-butoxycarbonyl)amino]methyl}-4-methoxyphenyl)-2-propenoic acid methyl ester

HRID 1296218

반응식

HRID 1296218 반응식
[CH:1]([C:3]1[CH:4]=[CH:5][C:6]([O:18][CH3:19])=[C:7]([CH:17]=1)[CH2:8][NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=O.[CH2:20]([O:27][C:28]([NH:30][CH:31](P(OC)(OC)=O)[C:32]([O-:34])=[O:33])=[O:29])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[CH2:41]1CCN2C(=NCCC2)CC1.C(OCC)(=O)C>ClCCl>[CH3:41][O:34][C:32](=[O:33])[C:31]([NH:30][C:28]([O:27][CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)=[O:29])=[CH:1][C:3]1[CH:4]=[CH:5][C:6]([O:18][CH3:19])=[C:7]([CH2:8][NH:9][C:10]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:16])[CH:17]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 22493931Tert-butyl (5-formyl-2-methoxybenzyl)carbamateHCID 131726531[(Benzyloxy)carbonyl]amino-2-(dimethoxyphosphoryl)acetate

생성물 1

HCID 694858062-{[(Benzyloxy)carbonyl]amino}-3-(3-{[(t-butoxycarbonyl)amino]methyl}-4-methoxyphenyl)-2-propenoic acid methyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2.65 g of t-butyl N-(5-formyl-2-methoxybenzyl)carbamate, 3.81 g of methyl 2-([(benzyloxy)carbonyl]amino-2-(dimethoxyphosphoryl)acetate and 1.75 g of 1,8-diazabicyclo[5,4,0]-7-undecene were dissolved in 50 ml of dichloromethane, followed by stirring for 15 hours at room temperature. 300 ml of ethyl acetate was added, and the organic layer was successively washed with 150 ml of water and 150 ml of brine, dried over magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography, and 4.09 g of 2-{[(benzyloxy)carbonyl]amino}-3-(3-{[(t-butoxycarbonyl)amino]methyl}-4-methoxyphenyl)-2-propenoic acid methyl ester was obtained as a colorless solid.

후처리

  1. washthe organic layer was successively washed with 150 ml of water and 150 ml of brine
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-0477333a245b4dbf88326acc3540545d
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244861B2

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