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Water → Aluminum,tris[2-[(acetyl-kO)oxy]benzoato-kO]-

HRID 1288430
ノート
印刷プレビュー

反応式

HRID 1288430 の反応式
C([Al:3](CC)CC)C.[C:8]([O:11][C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([O-:16])=[O:15])(=[O:10])[CH3:9].O>O1CCCC1>[C:8]([O:11][C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([O-:16])=[O:15])(=[O:10])[CH3:9].[C:8]([O:11][C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([O-:16])=[O:15])(=[O:10])[CH3:9].[C:8]([O:11][C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([O-:16])=[O:15])(=[O:10])[CH3:9].[Al+3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 3434975AcetylsalicylateHCID 16682930Triethylaluminum

生成物 1

HCID 10030780Aluminum,tris[2-[(acetyl-kO)oxy]benzoato-kO]-収率 88.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3.8 g of triethyl aluminum were dissolved in 70 ml of tetrahydrofuran. Under ice cooling, a solution of 10.8 g of o-acetoxybenzoate dissolved in 200 ml of tetrahydrofuran was added dropwise little by little to the above solution in nitrogen gas current. After completion of the dropwise addition, the temperature of the mixture was returned to room temperature, and it was thrown into a great quantity of water. The precipitated crude crystals were recovered by filtration and dried under reduced pressure to yield 10 g of white aluminum tris-(o-acetoxybenzoate) having a molecular weight of about 545 and an average degree of polymerization of about 1. The infrared absorption spectrum of the resulting salt was as follows:

後処理

  1. additionwas added dropwise little by little to the above solution in nitrogen gas current
  2. additionAfter completion of the dropwise addition
  3. customwas returned to room temperature
  4. customThe precipitated crude crystals
  5. filtrationwere recovered by filtration
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-4b45fcfcbeb64aa99d03835064a37c12
出典データセット
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03988333

反応ノート

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