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Trichloroisocyanuric Acid → HCID 20544433、化合物

HRID 2285842
ノート
印刷プレビュー

反応式

HRID 2285842 の反応式
[O:1]=[C:2]1[CH:7]=[C:6]([CH2:8][OH:9])[NH:5][CH:4]=[C:3]1[O:10][CH2:11][C:12]([OH:14])=[O:13].[Cl:15]N1C(=O)N(Cl)C(=O)N(Cl)C1=O>CO.O>[O:1]=[C:2]1[C:7]([Cl:15])=[C:6]([CH2:8][OH:9])[NH:5][CH:4]=[C:3]1[O:10][CH2:11][C:12]([OH:14])=[O:13]
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 2

HCID 6909Trichloroisocyanuric AcidHCID 20544454HCID 20544454、化合物

生成物 1

HCID 20544433HCID 20544433、化合物収率 121.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

2-(4-Oxo-6-hydroxymethyl-1,4-dihydropyridin-3-yloxy)acetic acid (5.97 g) was dissolved in a mixture of methanol (300 ml) and water (420 ml) at 65° to 70° C. and the solution was stirred at the same temperature. Trichloroisocyanuric acid (2.79 g) was added thereto, and the resultant mixture was stirred at the same temperature for 1.5 hours and then allowed to stand at room temperature over-night. The reaction mixture was cooled and the resulting crystals were collected by filtration, washed with water and dried. Thus obtained crystals (4.1 g) were recrystallized from water (100 ml) to give crystals (3.4 g) of 2-(4-oxo-5-chloro-6-hydroxymethyl-1,4-dihydropyridin-3-yloxy) acetic acid, mp 240° to 245° C.(dec).

後処理

  1. waitto stand at room temperature over-night
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe resulting crystals were collected by filtration
  4. washwashed with water
  5. customdried
  6. customThus obtained crystals (4.1 g) were recrystallized from water (100 ml)

出典と根拠

ORDレコード
ord-0bed78c286184b4ca7b48398e83d44fd
出典データセット
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04324892

反応ノート

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