Hydrochloric Acid → HCID 458355、化合物

HRID 1089184ノート

反応式

HRID 1089184 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 458355HCID 458355、化合物収率 72.6%

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-999d060c6e3842b0b4d4cd0bf99f358c
出典データセット
uspto-grants-1990_10
特許番号
US04965284

反応ノート

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