Potassium Hydroxide → HCID 14374020, 화합물

HRID 982543노트

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HRID 982543 반응식
[OH-].[K+].[OH:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([C:12]2[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=2)=[O:11])=[CH:6][CH:5]=1.[CH3:21][N:22]([CH3:26])[C:23](Cl)=[S:24]>O.O1CCCC1.[OH-].[Na+]>[CH3:21][N:22]([CH3:26])[C:23](=[S:24])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:11])[C:12]2[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=2)=[CH:6][CH:5]=1

참가 물질

7

반응물 3

HCID 14797Potassium HydroxideHCID 27871Dimethylthiocarbamoyl chlorideHCID 11096817(4-Hydroxyphenyl)(4-nitrophenyl)methanone

생성물 1

HCID 14374020HCID 14374020, 화합물수율 84%

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 14798Sodium Hydroxide용매

반응 조건

온도
50 °C

실험 절차

1.4 g (0.025 mol) of potassium hydroxide pellets are added to a suspension of 5.4 g (0.0224 mol) of 4-hydroxyphenyl 4-nitrophenyl methanone in 60 ml of water. The reaction mixture is heated at 50° C. for two hours, with vigorous stirring. The mixture is then cooled to 0° C. and a solution of 3.5 g (0.029 mol) of dimethylthiocarbamoyl chloride in 15 ml of tetrahydrofuran (THF) is added dropwise. When the addition is complete, the reaction mixture is stirred for 15 minutes at 0° C. and then for one hour at 20° C. The reaction medium is then hydrolyzed in 25 ml of 1N NaOH at 0° C. The precipitate obtained is filtered off and washed with water until the pH of the washings is neutral. After drying, it is recrystallized from a methylene chloride/hexane mixture to give 5.9 g (yield: 84%) of the expected product melting at 168° C.

후처리

  1. temperatureThe mixture is then cooled to 0° C.
  2. additionWhen the addition
  3. waitfor one hour at 20° C
  4. customat 0° C
  5. customThe precipitate obtained
  6. filtrationis filtered off
  7. washwashed with water until the pH of the washings
  8. customAfter drying
  9. customit is recrystallized from a methylene chloride/hexane mixture

출처 및 근거

ORD 기록
ord-7cd54d416d69404cb1fcefc6f1b82031
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04996347

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