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6-(2-Hydroxy-3-methoxypropyl)-9-methoxy-4-phenylpyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione → HCID 21980594, 화합물

HRID 11126
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HRID 11126 반응식
[OH:1][CH:2]([CH2:30][O:31]C)[CH2:3][N:4]1[C:16]2[CH:15]=[C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C:13]3[C:23](=[O:27])[NH:24][C:25](=[O:26])[C:12]=3[C:11]=2[C:10]2[CH:9]=[C:8]([O:28]C)[CH:7]=[CH:6][C:5]1=2>C(OCC)(=O)C.CCCCCC>[OH:1][CH:2]([CH2:30][OH:31])[CH2:3][N:4]1[C:16]2[CH:15]=[C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:13]3[C:23](=[O:27])[NH:24][C:25](=[O:26])[C:12]=3[C:11]=2[C:10]2[CH:9]=[C:8]([OH:28])[CH:7]=[CH:6][C:5]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

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반응물 1

HCID 219803456-(2-Hydroxy-3-methoxypropyl)-9-methoxy-4-phenylpyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione

생성물 1

HCID 21980594HCID 21980594, 화합물수율 31.6%

시약·촉매·용매 1

HCID 21226206Ethyl acetate hexane용매

실험 절차

Demethylation of alcohol (225) (96 mg, 0.22 mmol) prepared as described in example 290 employing the procedure described in example 80 was followed by chromatography on silica eluting with ethyl acetate/hexane (4:1). Crystallisation from ethyl acetate/hexane gave phenol (226) (28 mg, 31%) as an orange/yellow powder, mp 290–295° C. 1H NMR δ [(CD3)2SO] 11.04 (br s, 1H), 9.30 (s, 1H), 8.40 (d, J=2.4 Hz, 1H), 7.79 (s, 1H), 7.63 (m, 2H), 7.55 (d, J=8.8 Hz, 1H), 7.47 (m, 3H), 7.11 (dd, J=8.8, 2.4 Hz, 1H), 5.00 (d, J=5.4 Hz, 1H), 4.86 (t, J=5.4 Hz, 1H), 4.51 (dd, J=3.8, 14.9 Hz, 1H), 4.35 (dd, J=7.5, 14.9 Hz, 1H), 3.89 (m, 1H), 3.41 (m, 2H). Found: C, 67.94; H, 4.69; N, 6.50. C23H18N2O5.1/4H2O requires: C, 67.89; H, 4.58; N, 6.88.

후처리

  1. customCrystallisation from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-b5ff531db69c462a869d3c4a2037c1a7
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07094798B1

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