Ammonia → HCID 14601662、化合物

HRID 1638290ノート

反応式

HRID 1638290 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]3[CH2:19][CH2:18][CH:17]([OH:20])[CH2:16][CH2:15]3)=[O:13])[C:6]=2[CH:21]=1.[C:22](Cl)(Cl)=[O:23].[NH3:26]>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]3[CH2:15][CH2:16][CH:17]([O:20][C:22](=[O:23])[NH2:26])[CH2:18][CH2:19]3)=[O:13])[C:6]=2[CH:21]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 6371PhosgeneHCID 3082453Hpr 611

生成物 1

HCID 14601662HCID 14601662、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of 5-chloro-3-(4-hydroxypiperidinocarbonylmethyl)benzothiazolin-2-one (3.2 g) in dry dioxane (70 ml) was gradually dropped in a phosgene solution in dry dioxane (10 ml), under cooling. The mixture was left for two hours at room temperature. After cooling, to the mixture was gradually dropwise added 28% aqueous ammonia (5 ml) and the resultant was stirred for two hours at room temperature. Dioxane was evaporated off under vacuum from the reaction mixture. The residue was washed with water and then recrystallized from a mixture of dioxane and ethanol to yield the title compound as colorless crystals (2.8 g). m.p. 210°-212° C.

後処理

  1. temperatureunder cooling
  2. temperatureAfter cooling, to the mixture
  3. customDioxane was evaporated off under vacuum from the reaction mixture
  4. washThe residue was washed with water
  5. customrecrystallized from a mixture of dioxane and ethanol

出典と根拠

ORDレコード
ord-2ca16ae4225a4719995a1777bf5e5d9b
出典データセット
uspto-grants-1989_11
特許番号
US04879301

反応ノート

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