Acetic Acid → HCID 178508855、化合物

HRID 2259445ノート

反応式

HRID 2259445 の反応式
[NH2:1][C:2]1[N:3]=[C:4]([OH:24])[C:5]2[CH:11]=[C:10]([CH2:12][CH2:13][C:14]3[CH:23]=[CH:22][C:17]([C:18]([O:20]C)=[O:19])=[CH:16][CH:15]=3)[CH:9]=[N:8][C:6]=2[N:7]=1.[OH-].[Na+].C(O)(=O)C.O>CO>[NH2:1][C:2]1[N:3]=[C:4]([OH:24])[C:5]2[CH:11]=[C:10]([CH2:12][CH2:13][C:14]3[CH:23]=[CH:22][C:17]([C:18]([OH:20])=[O:19])=[CH:16][CH:15]=3)[CH:9]=[N:8][C:6]=2[N:7]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 178497708HCID 178497708、化合物

生成物 1

HCID 178508855HCID 178508855、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 0.46 g of methyl 4-[2-(2-amino-4-hydroxypyrido[2,3,d]pyrimidin-6-yl)ethyl]benzoate and 30 mL of 1N sodium hydroxide is stirred at room temperature for 36 hours and then acidified with glacial acetic acid. The resulting suspension is centrifuged with fresh water several times and then combined with methanol. The water is removed azeotropically under reduced pressure to yield 4-[2-(2-amino-4-hydroxypyrido[2,3-d]pyrimidin-6-yl)ethyl]benzoic acid, m.p. >300° C.; IR (KBr) ν max 3220, 2855, 1680, 1607, 1483, 1398, 1253, 1179, 1016, and 812 cm-1 ; 1H NMR (dTFA, d6DMSO) delta 8.38 (s, 1H (7)-H), 8.02 (s, 1H, (5)-H), 7.62 (d, J=8.0 Hz, 2H, Ar), 6.87 (s, 1H, (3)-H), 6.82 (d, J=8.0 Hz, 2H, Ar), 2.79 (m, 2H, (6)-CH2 --), 2.70 (m, 2H, benzyl).

後処理

  1. customThe water is removed azeotropically under reduced pressure

出典と根拠

ORDレコード
ord-7f089613825d4323b95b1228e47d22d8
出典データセット
uspto-grants-1995_12
特許番号
US05473071

反応ノート

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