Hydrochloric Acid → HCID 14461232, 화합물

HRID 2351865노트

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HRID 2351865 반응식
O1COCO[CH2:2]1.[CH:7]1[CH:12]=[CH:11][C:10]([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=2)=[CH:9][CH:8]=1.[ClH:24]>[Cl-].[Zn+2].[Cl-].C(O)(=O)C>[Cl:24][CH2:2][C:7]1[CH:8]=[CH:9][C:10]([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:21])([F:22])[F:23])=[CH:16][CH:15]=2)=[CH:11][CH:12]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 80811,3,5-Trioxane2회HCID 5976471-Benzyl-4-(trifluoromethyl)benzene

생성물 1

HCID 14461232HCID 14461232, 화합물수율 20%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매2회HCID 176Acetic Acid용매

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온도
60 °C

실험 절차

In a 250 ml of round-bottom three-necked flask, 0.68 g of zinc chloride (dried for 3 hours under vacuum at 100° C.); 4.0 g of 1,3,5-trioxane; 16.0 g of 4-trifluoromethyldiphenylmethane and 4.5 ml of 100% acetic acid are combined, heated to 60° C. and dried halogen chloride gas is introduced. The result is a two phase system that turns brown. HCl was introduced for a total of 3 hours. Following 6 hours of reaction time, the conversion is d.c. controlled (developing agent: petroleum benzin 60°-80° C., result: no conversion, starting material). Once again 0.68 g of ZnCl2 and 2.0 g of 1,3,5-trioxane are added to the reaction mixture and stirred overnight. The reaction mixture was stirred for a total of 30 hours at 60° C., whereby following dc result, approximately 20% of the desired compound formed. The mixture was cooled to room temperature and diluted with 150 ml of diethyl ether. The ether solution was washed to neutral several times with a total of 2.5 liters of water. The organic phase was shaken once with 80 ml of a saturated sodium hydrogen carbonate solution and then washed to neutral 2 times with 90 ml of water each time. The organic phase was dried over sodium sulfate. The drying agent was removed by filtration and the filtrate was concentrated in a rotary evaporator (30° C., water-jet vacuum).

후처리

  1. customFollowing 6 hours of reaction time
  2. stirringThe reaction mixture was stirred for a total of 30 hours at 60° C.

출처 및 근거

ORD 기록
ord-d0cd0faccd0947b9b21224e962d1811b
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04874763

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