Water → HCID 11360577、化合物

HRID 1833274ノート

反応式

HRID 1833274 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]([C:15](=[O:24])[C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH3:23])[CH:17]=1)=[N:8][CH:7]=[C:6]2[C:25](O)=[O:26].[Cl-].[NH4+].C([N:32](CC)CC)C.O>CN(C)C=O.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]([C:15](=[O:24])[C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH3:23])[CH:17]=1)=[N:8][CH:7]=[C:6]2[C:25]([NH2:32])=[O:26]

参加物

7

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 11394498HCID 11394498、化合物

生成物 1

HCID 11360577HCID 11360577、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 6,7-dimethoxy-1-(3-methoxy-benzoyl)-isoquinoline-4-carboxylic acid (30mg, 81.7 mmol), ammonium chloride (43.5 mg. 0.817 mM) and triethylamine (0.115 mL, 0.817 mM) in 2 mL of dimethylformamide was stirred with O-benzotriazol-1-yl-N,N,N,N-tetramethyluronium hexafluorophosphate (61.9 mg. 0.163 mM) at room temperature for 20 hours. Poured into 20 mL of water and 20 mL of ethyl acetate, extracted ethyl acetate layer with saturated sodium bicarbonate, dried ethyl acetate solution. over anhydrous magnesium sulfate and evaporated to give 5.4 mg of an off-white solid pure product: APCI-MS m/e calcd for C20H18N2O6 (M+H.) 367.4, found 367; H NMR (300 MHz) compatible.

後処理

  1. extractionextracted ethyl acetate layer with saturated sodium bicarbonate, dried ethyl acetate solution
  2. customover anhydrous magnesium sulfate and evaporated

出典と根拠

ORDレコード
ord-ae5c0f2fddc7429690556430f9b1672d
出典データセット
uspto-grants-2006_06
特許番号
US07067529B2

反応ノート

読み込み中…