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Hydrochloric Acid → 2-Amino-5-chloro-4-(4-pyridylthiomethyl)thiazole

HRID 1656969
ノート
印刷プレビュー

反応式

HRID 1656969 の反応式
[Cl:1][C:2]1[S:6][C:5]([NH:7]C=O)=[N:4][C:3]=1[CH2:10][S:11][C:12]1[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=1.O1CCCC1.Cl>C(O)C>[NH2:7][C:5]1[S:6][C:2]([Cl:1])=[C:3]([CH2:10][S:11][C:12]2[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=2)[N:4]=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 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 157291695-Chloro-2-formylamino-4-(4-pyridylthiomethyl)thiazole

生成物 1

HCID 189547322-Amino-5-chloro-4-(4-pyridylthiomethyl)thiazole収率 56.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 5-chloro-2-formylamino-4-(4-pyridylthiomethyl)thiazole (4.9 g) in a mixture of ethanol (25 ml), tetrahydrofuran (20 ml) and concentrated hydrochloric acid (7 ml) was stirred at room temperature for 4 hours. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in water. The solution was adjusted to pH 8 using aqueous sodium bicarbonate under ice-cooling. The precipitates were collected by filtration, washed with water and dried in vacuo to give 2-amino-5-chloro-4-(4-pyridylthiomethyl)thiazole (0.26 g, yield: 56.6%). IR (Nujol): 3350, 3250, 1685, 1530 cm-1

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in water
  3. temperaturecooling
  4. filtrationThe precipitates were collected by filtration
  5. washwashed with water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-d3dc3efbfdc34ac99a0f3d9f276a44d1
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05256675

反応ノート

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