Formic Acid → HCID 59540634, 화합물

HRID 1677492노트

반응식

HRID 1677492 반응식
[OH:1][CH:2]1[CH2:7][CH2:6][C:5]([C:9]([C:11]2[C:19]3[C:14](=[N:15][CH:16]=[C:17]([C:20]4[CH:25]=[C:24]([O:26][CH3:27])[C:23]([O:28][CH3:29])=[C:22]([O:30][CH3:31])[CH:21]=4)[N:18]=3)[NH:13][CH:12]=2)=[O:10])([CH3:8])[CH2:4][CH2:3]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH:51](O)=[O:52].N(C(OCC)=O)=NC(OCC)=O>C1COCC1>[CH3:8][C:5]1([C:9]([C:11]2[C:19]3[C:14](=[N:15][CH:16]=[C:17]([C:20]4[CH:21]=[C:22]([O:30][CH3:31])[C:23]([O:28][CH3:29])=[C:24]([O:26][CH3:27])[CH:25]=4)[N:18]=3)[NH:13][CH:12]=2)=[O:10])[CH2:4][CH2:3][CH:2]([O:1][CH:51]=[O:52])[CH2:7][CH2:6]1

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 59540549HCID 59540549, 화합물

생성물 1

HCID 59540634HCID 59540634, 화합물수율 59%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of (4-hydroxy-1-methyl-cyclohexyl)-[2-(3,4,5-trimethoxy-phenyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl]-methanone (19 mg, 0.045 mmol), triphenyl phosphine (23 mg, 0.088 mmol), and formic acid (0.003 ml, 0.087 mmol), in THF (0.4 ml), was treated with diethyl azodicarboxylate (0.01 ml, 0.092 mmol). After stirring at room temperature for 2 days, the reaction mixture was purified by preparative thin layer chromatography using 70% EtOAc in Hexanes as eluant providing 12 mg (59%) of formic acid 4-methyl-4-[2-(3,4,5-trimethoxy-phenyl)-5H-pyrrolo[2,3-b]pyrazine-7-carbonyl]-cyclohexyl ester as a white solid. M+H=454.

후처리

  1. customthe reaction mixture was purified by preparative thin layer chromatography

출처 및 근거

ORD 기록
ord-29a66d1c0508440faa36329f0e2dc67f
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08008298B2

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