Water → HCID 11360577, 화합물

HRID 1833274노트

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HRID 1833274 반응식
[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]

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 11394498HCID 11394498, 화합물

생성물 1

HCID 11360577HCID 11360577, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-ae5c0f2fddc7429690556430f9b1672d
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07067529B2

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