Water → Sbb012730

HRID 839095

반응식

HRID 839095 반응식
O.[C:2](Cl)(Cl)=[S:3].[NH2:6][C:7]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:8]=1[C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:10]>C(Cl)Cl>[C:9]([C:8]1[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:7]=1[N:6]=[C:2]=[S:3])(=[O:10])[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

5

반응물 3

HCID 962Water2회HCID 10040ThiophosgeneHCID 128702-Amino-5-chlorobenzophenone

생성물 1

HCID 5200219Sbb012730

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A five liter, 3-necked, round-bottom flask equipped with a condenser plus scrubber, mechanical stirrer, and dropping funnel was used as the reaction vessel. The reaction vessel was cooled in an ice bath after charging with 1.2 liters of water. After the water had cooled, 126 ml (1.65 moles) of thiophosgene was added. The mixture was stirred vigorously while a solution containing 352 grams (1.52 moles) of 2-amino-5-chlorobenzophenone in about 1 liter of methylene chloride was added over a period of 20 to 25 minutes. After addition was complete the funnel was rinsed with about 150 ml of methylene chloride and the reaction mixture was stirred for about one hour with the ice bath in place. Then the ice bath was removed and the reaction mixture was stirred for one additional hour. The organic phase was separated, dried with magnesium sulfate, and concentrated in vacuo. The 2-benzoyl-4-chlorophenylisothiocyanate remained behind as a brown oil which solidified on cooling. The product was recrystallized from hexane to yield tan crystals.

후처리

  1. customA five liter, 3-necked, round-bottom flask equipped with a condenser
  2. temperatureThe reaction vessel was cooled in an ice bath
  3. additionwas added over a period of 20 to 25 minutes
  4. additionAfter addition
  5. washwas rinsed with about 150 ml of methylene chloride
  6. stirringthe reaction mixture was stirred for about one hour with the ice bath in place
  7. customThen the ice bath was removed
  8. stirringthe reaction mixture was stirred for one additional hour
  9. customThe organic phase was separated
  10. dry with materialdried with magnesium sulfate
  11. concentrationconcentrated in vacuo
  12. temperatureon cooling
  13. customThe product was recrystallized from hexane
  14. customto yield tan crystals

출처 및 근거

ORD 기록
ord-ea2e6990e7db42debb582158a7b75b0d
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093805

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