Diisopropylethylamine → {2-[(4'-Octyloxy-biphenyl-4-carbonyl)-amino]-benzyl}-phosphonic acid diethylester

HRID 1642062노트

반응식

HRID 1642062 반응식
[CH2:1]([O:3][P:4]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH2:16])(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[CH2:17]([O:25][C:26]1[CH:31]=[CH:30][C:29]([C:32]2[CH:37]=[CH:36][C:35]([C:38](O)=[O:39])=[CH:34][CH:33]=2)=[CH:28][CH:27]=1)[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24].CCN(C(C)C)C(C)C.C1C=NC2N(O)N=NC=2C=1>CN(C=O)C.CCOC(C)=O.C(Cl)CCl>[CH2:6]([O:5][P:4]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH:16][C:38]([C:35]1[CH:34]=[CH:33][C:32]([C:29]2[CH:30]=[CH:31][C:26]([O:25][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:27][CH:28]=2)=[CH:37][CH:36]=1)=[O:39])(=[O:8])[O:3][CH2:1][CH3:2])[CH3:7]

참가 물질

8

반응물 4

HCID 81531DiisopropylethylamineHCID 181649HOAtHCID 28025564'-(Octyloxy)-[1,1'-biphenyl]-4-carboxylic acidHCID 13649220Diethyl [(2-aminophenyl)methyl]phosphonate

생성물 1

HCID 86638333{2-[(4'-Octyloxy-biphenyl-4-carbonyl)-amino]-benzyl}-phosphonic acid diethylester

시약·촉매·용매 3

HCID 111,2-Dichloroethane용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

1 g of (2-amino-benzyl)-phosphonic acid diethyl ester, 2 g of 4′-octyloxy-biphenyl-4-carboxylic acid, 1.4 ml of EDC, 0.9 ml of DIEA and 100 mg of HOAt are dissolved in 30 ml of DMF and the mixture obtained is stirred at rt for 2 days. The mixture obtained is diluted with EtOAc and the solution obtained is washed with aqueous diluted HCl and aqueous NaHCO3 solution. The organic layer obtained is dried and solvent is evaporated. {2-[(4′-Octyloxy-biphenyl-4-carbonyl)-amino]-benzyl}-phosphonic acid diethylester is obtained in crystalline form and is recrystallized from iso-propanol/water.

후처리

  1. customthe mixture obtained
  2. customThe mixture obtained
  3. customthe solution obtained
  4. washis washed with aqueous diluted HCl and aqueous NaHCO3 solution
  5. customThe organic layer obtained
  6. customis dried
  7. customsolvent is evaporated

출처 및 근거

ORD 기록
ord-310c25592dd84c46b45f0c5c1a7438c8
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119617B2

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