Formic Acid → HCID 59540634、化合物

HRID 1677492ノート

反応式

HRID 1677492 の反応式
[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

参加物

6

反応物 4

HCID 284Formic AcidHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 59540549HCID 59540549、化合物

生成物 1

HCID 59540634HCID 59540634、化合物収率 59%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-29a66d1c0508440faa36329f0e2dc67f
出典データセット
uspto-grants-2011_08
特許番号
US08008298B2

反応ノート

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