Hydrochloric Acid → HCID 458355, 화합물

HRID 1089184노트

반응식

HRID 1089184 반응식
[CH3:1][C:2]([C:4]1[CH:16]=[CH:15][C:7]2[S:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[C:6]=2[CH:5]=1)=[O:3].[Cl-].[Al+3].[Cl-].[Cl-].[C:21](Cl)(=[O:23])[CH3:22].Cl>C(=S)=S>[C:21]([C:12]1[CH:13]=[CH:14][C:9]2[S:8][C:7]3[CH:15]=[CH:16][C:4]([C:2](=[O:3])[CH3:1])=[CH:5][C:6]=3[C:10]=2[CH:11]=1)(=[O:23])[CH3:22]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 3120271-(Dibenzo[b,d]thiophen-2-yl)ethan-1-oneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 458355HCID 458355, 화합물수율 72.6%

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

To a solution of 45.3 g of 2-dibenzothienyl methyl ketone in one liter of carbon disulfide was added 106 g of anhydrous aluminum chloride. To this was added 17.3 g of acetyl chloride over 8 minutes. This mixture was refluxed for 3 hours and then poured into a mixture of 2 liters of crushed ice and 400 ml of concentrated hydrochloride acid. This mixture was stirred until the green color had changed to pale tan, then the solid was collected washed with water and air dried. This solid was collected, washed with water and air dried. This solid was dissolved in 2 liters of hot acetontride, filtered, concentrated to about one liter and allowed to crystallize, giving 39.0 g of the desired product as tan crystals, mp 207°-210° C.

후처리

  1. temperatureThis mixture was refluxed for 3 hours
  2. customthe solid was collected
  3. washwashed with water and air
  4. customdried
  5. customThis solid was collected
  6. washwashed with water and air
  7. customdried
  8. dissolutionThis solid was dissolved in 2 liters of hot acetontride
  9. filtrationfiltered
  10. concentrationconcentrated to about one liter
  11. customto crystallize

출처 및 근거

ORD 기록
ord-999d060c6e3842b0b4d4cd0bf99f358c
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04965284

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