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Hydrochloric Acid → HCID 54724773、化合物

HRID 2216423
ノート
印刷プレビュー

反応式

HRID 2216423 の反応式
[OH:1][C:2]1[C:10]2[C:5](=[N:6][C:7]([CH:11]([CH3:13])[CH3:12])=[CH:8][CH:9]=2)[S:4][C:3]=1[C:14]([O:16]C)=O.[NH2:18][C:19]1[CH:20]=[CH:21][C:22]([O:27][CH2:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[C:23]([CH:26]=1)[C:24]#[N:25].Cl>>[C:24]([C:23]1[CH:26]=[C:19]([NH:18][C:14]([C:3]2[S:4][C:5]3=[N:6][C:7]([CH:11]([CH3:12])[CH3:13])=[CH:8][CH:9]=[C:10]3[C:2]=2[OH:1])=[O:16])[CH:20]=[CH:21][C:22]=1[O:27][CH2:28][C:29]([CH3:31])([CH3:30])[CH3:32])#[N:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 178227345-Amino-2-neopentyloxybenzonitrileHCID 54724774HCID 54724774、化合物

生成物 1

HCID 54724773HCID 54724773、化合物収率 22.3%

実験手順

Methyl 3-hydroxy-6-isopropylthieno[2,3-b]pyridine-2-carboxylate (1.6 g) and 5-amino-2-neopentyloxybenzonitrile (2.6 g) were stirred at 170° C. for 2 hr. Then the reaction mixture was treated with diluted hydrochloric acid and the organic layer was extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained crystals were recrystallized from water-containing dimethylformamide to give the title compound (0.6 g). melting point: 211-212° C.

後処理

  1. extractionthe organic layer was extracted with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customThe obtained crystals were recrystallized from water-
  6. additioncontaining dimethylformamide

出典と根拠

ORDレコード
ord-5d00f2f0461a48839d5645515385459e
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07112594B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート