Methyl isothiocyanate → HCID 178488243、化合物

HRID 500544ノート

反応式

HRID 500544 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][N:12]=1)[C:6]([NH:8][NH2:9])=O.[CH3:13][N:14]=[C:15]=[S:16].[OH-].[Na+]>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:6]2[N:14]([CH3:13])[C:15]([SH:16])=[N:9][N:8]=2)[CH:10]=[CH:11][N:12]=1

参加物

5

反応物 3

HCID 11167Methyl isothiocyanateHCID 14798Sodium HydroxideHCID 3225512-Methoxyisonicotinohydrazide

生成物 1

HCID 178488243HCID 178488243、化合物収率 87%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

The title compound of example 23.1 (18.35 g, 109.8 mmol) and methyl isothiocyanate (8.83 g, 120 mmol) were stirred together at 60° C. for 30 minutes. Sodium hydroxide (4.83 g, 120 mmol) in water (32 mL) was added to the reaction mixture it was allowed to continue to stir at 60° C. for 12 hours. The reaction mixture was concentrated and diluted with water. It was acidified to pH 4-5 with 3 M HCl. A solid precipitated out which was filtered, washing with portions of water, then dried to afford the product as a beige solid (21.2 g, 87%).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with water
  3. customA solid precipitated out which
  4. filtrationwas filtered
  5. washwashing with portions of water
  6. customdried

出典と根拠

ORDレコード
ord-c51b3d4008d2404abf5a551ade3cdcf0
出典データセット
uspto-grants-2010_08
特許番号
US07772235B2

反応ノート

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