3,5-Diaminobenzoic acid → Benzoic Acid

HRID 416202

反応式

HRID 416202 の反応式
N[C:2]1[CH:3]=[C:4]([CH:8]=[C:9](N)[CH:10]=1)[C:5]([OH:7])=[O:6].C(N(CC)C(C)C)(C)C>CN(C=O)C>[C:5]([OH:7])(=[O:6])[C:4]1[CH:8]=[CH:9][CH:10]=[CH:2][CH:3]=1

参加物

4

反応物 2

HCID 120623,5-Diaminobenzoic acidHCID 81531Diisopropylethylamine

生成物 1

HCID 243Benzoic Acid

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3,5-Diaminobenzoic acid (4.3 mg, 0.028 mmol, 0.40 equiv.) was dissolved in 10 mL of anhydrous DMF. To the solution was added H-PEOZ-p-NPC 10K (1.00 gm, 0.0692 mmol, 1.0 equiv.; an active NHS ester can also be used), followed by addition of N,N-Diisopropylethyl amine (DIPEA, 36.2 μL, 0.208 mmol, 3.0 equiv.). Following overnight stirring at room temperature, the solution was evaporated to dryness by rotary evaporation under vacuum at 50° C. The residue was dissolved in dichloromethane, and then precipitated by addition into diethyl ether with stirring. The precipitate was filtered and dried under vacuum. The molecular weight of H-PEOZ2-benzoic acid was verified by GPC.

後処理

  1. customthe solution was evaporated to dryness by rotary evaporation under vacuum at 50° C
  2. dissolutionThe residue was dissolved in dichloromethane
  3. customprecipitated by addition into diethyl ether
  4. stirringwith stirring
  5. filtrationThe precipitate was filtered
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-a9443d056c6f4e3390c8196cd49be22f
出典データセット
uspto-grants-2012_01
特許番号
US08088884B2

関連ノート

読み込み中…