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

HRID 1642062ノート

反応式

HRID 1642062 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-310c25592dd84c46b45f0c5c1a7438c8
出典データセット
uspto-grants-2012_02
特許番号
US08119617B2

反応ノート

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