Ammonia → HCID 14601662, 화합물

HRID 1638290노트

반응식

HRID 1638290 반응식
[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

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 6371PhosgeneHCID 3082453Hpr 611

생성물 1

HCID 14601662HCID 14601662, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2ca16ae4225a4719995a1777bf5e5d9b
출처 데이터셋
uspto-grants-1989_11
특허 번호
US04879301

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