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Methanol → HCID 18399215, 화합물

HRID 1019370
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HRID 1019370 반응식
C([O:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13]([C:30]3[CH:35]=[C:34]([O:36][CH3:37])[C:33]([O:38][CH3:39])=[C:32]([O:40][CH3:41])[CH:31]=3)=[C:14]([C:26]([O:28][CH3:29])=[O:27])[N:15]([N:20]3[CH2:25][CH2:24][O:23][CH2:22][CH2:21]3)[C:16]2=[O:19])=[CH:11][C:10]=1[O:42][CH3:43])C1C=CC=CC=1.CO>[C].[Pd].CN(C)C=O>[OH:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13]([C:30]3[CH:35]=[C:34]([O:36][CH3:37])[C:33]([O:38][CH3:39])=[C:32]([O:40][CH3:41])[CH:31]=3)=[C:14]([C:26]([O:28][CH3:29])=[O:27])[N:15]([N:20]3[CH2:21][CH2:22][O:23][CH2:24][CH2:25]3)[C:16]2=[O:19])=[CH:11][C:10]=1[O:42][CH3:43]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 887MethanolHCID 18399330HCID 18399330, 화합물

생성물 1

HCID 18399215HCID 18399215, 화합물수율 95.2%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 6228Dimethylformamide용매

실험 절차

To the compound obtained in Example 1 (2.8 g) are added methanol (100 ml), dimethylformamide (100 ml) and palladium-carbon (100 mg), and the mixture is stirred under hydrogen atmosphere (1 atm) at room temperature for 1.5 hour. The catalyst is removed by filtration, and the filtrate is concentrated. The precipitated crystals are collected by filtration, and washed with diethyl ether to give 7-hydroxy-6-methoxy-3-methoxycarbonyl-2-morpholino-4-(3,4,5-trimethoxyphenyl)-1(2H)-isoquinolinone (2.26 g) as listed in Table 1.

후처리

  1. customThe catalyst is removed by filtration
  2. concentrationthe filtrate is concentrated
  3. filtrationThe precipitated crystals are collected by filtration
  4. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-478bbd789fe24d5db67ba59443b47364
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06486155B1

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