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Chloroacetone → 5-chloro-N-(4-methylthiazol-2-yl)-3-phenoxypyridin-2-amine

HRID 335076
ノート
印刷プレビュー

反応式

HRID 335076 の反応式
Cl[CH2:2][C:3](=O)[CH3:4].[Cl:6][C:7]1[CH:8]=[C:9]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:10]([NH:13][C:14]([NH2:16])=[S:15])=[N:11][CH:12]=1.C(N(CC)CC)C>C(O)C>[Cl:6][C:7]1[CH:8]=[C:9]([O:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:10]([NH:13][C:14]2[S:15][CH:2]=[C:3]([CH3:4])[N:16]=2)=[N:11][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6571ChloroacetoneHCID 8471TriethylamineHCID 866314681-(5-Chloro-3-phenoxypyridin-2-yl)thiourea

生成物 1

HCID 247655385-chloro-N-(4-methylthiazol-2-yl)-3-phenoxypyridin-2-amine収率 88.96%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1-chloropropan-2-one (3.827 g, 41.36 mmol), 1-(5-chloro-3-phenoxypyridin-2-yl)thiourea (8.265 g, 29.54 mmol), triethylamine (7.001 mL, 50.23 mmol), and ethanol (30 mL) was refluxed for 3 hours. The ethanol was removed to about one third original volume, and then the reaction mixture was cooled in an ice bath and filtered. The solids were washed with cold ethanol and dried to afford the title compound (8.35 g, 88.96% yield) as a light yellow powder. 1H NMR (d6-DMSO) δ 10.94 (bs, 1H), 8.15 (d, 1H), 7.43 (t, 2H), 7.32 (d, 1H), 7.20 (t, 1H), 7.19 (d, 2H), 6.60 (s, 1H), 2.23 (s, 3H); Mass spectrum (apci) m/z=318.2 (M+H).

後処理

  1. temperaturewas refluxed for 3 hours
  2. customThe ethanol was removed to about one third original volume
  3. temperaturethe reaction mixture was cooled in an ice bath
  4. filtrationfiltered
  5. washThe solids were washed with cold ethanol
  6. customdried

出典と根拠

ORDレコード
ord-66d48826788245de8658e52969c2258d
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883828B2

反応ノート

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