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Ethyl Acetate → HCID 18399146, 화합물

HRID 1019371
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HRID 1019371 반응식
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([C:23]3[CH:28]=[C:27]([O:29][CH3:30])[C:26]([O:31][CH3:32])=[C:25]([O:33][CH3:34])[CH:24]=3)=[C:7]([C:19]([O:21][CH3:22])=[O:20])[N:8]([N:13]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)[C:9]2=[O:12])=[CH:4][C:3]=1[O:35][CH3:36].Cl.[N:38]1[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=1[CH2:44][Cl:45].C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CN(C)C=O.O>[ClH:45].[CH3:36][O:35][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:2]=1[O:1][CH2:44][C:39]1[CH:40]=[CH:41][CH:42]=[CH:43][N:38]=1)[C:9](=[O:12])[N:8]([N:13]1[CH2:14][CH2:15][O:16][CH2:17][CH2:18]1)[C:7]([C:19]([O:21][CH3:22])=[O:20])=[C:6]2[C:23]1[CH:28]=[C:27]([O:29][CH3:30])[C:26]([O:31][CH3:32])=[C:25]([O:33][CH3:34])[CH:24]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 23392Picolyl chloride hydrochlorideHCID 18399215HCID 18399215, 화합물

생성물 1

HCID 18399146HCID 18399146, 화합물수율 74.1%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

To a solution of the compound obtained in Example 2 (300 mg) in dimethylformamide (3 ml) are added 2-picolyl chloride hydrochloride (118 mg) and potassium carbonate (182 mg), and the mixture is stirred at 50° C. overnight. To the mixture are added ethyl acetate and water. The ethyl acetate layer is separated, washed, dried, and concentrated under reduced pressure. The residue (chemical name; 6-methoxy-3-methoxycarbonyl-2-morpholino-7-(2-pyridylmethyloxy)-4-(3,4,5-trimethoxyphenyl-1(2H)-isoquinolinone) is dissolved in ethyl acetate, and thereto is added a 4M solution of hydrogen chloride in ethyl acetate (150 μl). The mixture is stirred at room temperature for 30 minutes. The precipitated crystals are collected by filtration, and washed with ethyl acetate to give 6-methoxy-3-methoxycarbonyl-2-morpholino-7-(2-pyridylmethyloxy)-4-(3,4,5-trimethoxyphenyl)-1(2H)-isoquinolinone hydrochloride (279 mg) as listed in Table 1.

후처리

  1. customThe ethyl acetate layer is separated
  2. washwashed
  3. customdried
  4. concentrationconcentrated under reduced pressure
  5. dissolution6-methoxy-3-methoxycarbonyl-2-morpholino-7-(2-pyridylmethyloxy)-4-(3,4,5-trimethoxyphenyl-1(2H)-isoquinolinone) is dissolved in ethyl acetate
  6. additionis added a 4M solution of hydrogen chloride in ethyl acetate (150 μl)
  7. stirringThe mixture is stirred at room temperature for 30 minutes
  8. filtrationThe precipitated crystals are collected by filtration
  9. washwashed with ethyl acetate

출처 및 근거

ORD 기록
ord-6037f1167e2142f39ac0fd73753f3b0d
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06486155B1

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