3-(6-Chloropyrimidin-4-yl)benzoic acid → HCID 69486856、化合物

HRID 498250ノート

反応式

HRID 498250 の反応式
CO[C:3](=[O:21])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]2[CH:15]=[C:14]([NH:16][CH2:17][CH2:18][O:19][CH3:20])[N:13]=[CH:12][N:11]=2)[CH:5]=1.ClC1N=CN=C(C2C=[C:31](C=CC=2)[C:32]([OH:34])=[O:33])C=1>COCCN>[C:4]([O:34][C:32](=[O:33])[CH2:31][C:3]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]2[CH:15]=[C:14]([NH:16][CH2:17][CH2:18][O:19][CH3:20])[N:13]=[CH:12][N:11]=2)[CH:5]=1)=[O:21])([CH3:9])([CH3:5])[CH3:3]

参加物

4

反応物 2

HCID 223175383-(6-Chloropyrimidin-4-yl)benzoic acidHCID 694899033-[6-(2-Methoxy-ethylamino)-pyrimidin-4-yl]-benzoic acid methyl ester

生成物 1

HCID 69486856HCID 69486856、化合物

試薬・触媒・溶媒 1

HCID 80182-Methoxyethylamine溶媒

反応条件

温度
50 °C

実験手順

The title compound was prepared from 3-[6-(2-methoxy-ethylamino)-pyrimidin-4-yl]-benzoic acid methyl ester [prepared by the following procedure: 3-(6-Chloro-pyrimidin-4-yl)-benzoic acid (1.0 g, 4.3 mmol) was heated in 2-methoxy-ethylamine (5 ml) to 80° C. for 1 h. The mixture was evaporated in vacuum and the residual oil was stirred in 1N HCl-MeOH (25 mL) for 18 h at 50° C. The crude product was purified by chromatography (silica gel, AcOEt-hexane 1:1) to give the methyl ester as light yellow solid (0.67 g).] (0.66 g, 2.3 mmol) by treatment with lithium tert-butyl acetate according to general procedure K (method b). Obtained as a light yellow oil (0.93 g, not pure).

後処理

  1. customprepared by the following procedure
  2. customThe mixture was evaporated in vacuum
  3. customThe crude product was purified by chromatography (silica gel, AcOEt-hexane 1:1)

出典と根拠

ORDレコード
ord-c12ea2c5349f49d991bf7a2a6670ae5b
出典データセット
uspto-grants-2005_09
特許番号
US06949542B2

反応ノート

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