3-Nitrophenylboronic Acid → HCID 178514280、化合物

HRID 343991ノート

反応式

HRID 343991 の反応式
[NH2:1][NH:2][C:3]([NH:5][NH2:6])=[S:4].[N+:7]([C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH2:20][CH3:21])C(O)=O)=[CH:12][CH:11]=1)([O-:9])=[O:8].[N+]([C:25]1C=C(B(O)O)C=CC=1)([O-])=O>C1(C)C=CC=CC=1>[NH2:6][N:5]1[C:3]([SH:4])=[N:2][N:1]=[C:25]1[CH2:21][CH2:20][CH2:16][C:13]1[CH:12]=[CH:11][C:10]([N+:7]([O-:9])=[O:8])=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 16773-Nitrophenylboronic AcidHCID 240472-(4-Nitrophenyl)butyric acidHCID 2724189Thiocarbohydrazide

生成物 1

HCID 178514280HCID 178514280、化合物収率 647.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a mixture of 4.9 g (47 mmol) of thiocarbohydrazide and 9.8 g (47 mmol) of 4-nitrophenylbutanoic acid in 30 mL of toluene was added 0.8 g (4.7 mmol) of 3-nitrobenzeneboronic acid. The mixture was heated at reflux for 24 hr. The reaction was cooled and the reaction mixture was allowed to settle. The supernatant liquid was decanted. To the residual solid was added 50 mL of acetonitrile. The mixture was stirred for 30 minutes. The solid was collected, rinsed with 10 mL of acetonitrile and dried in vacuo to yield 8.5 g (65.4%) of the desired product as a white sandy material. All the analytical data confirmed the assigned structure.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 24 hr
  3. temperatureThe reaction was cooled
  4. customThe supernatant liquid was decanted
  5. additionTo the residual solid was added 50 mL of acetonitrile
  6. customThe solid was collected
  7. washrinsed with 10 mL of acetonitrile
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-61054827c0584a55a09e22bc7caebfdd
出典データセット
uspto-grants-1999_01
特許番号
US05864042

反応ノート

読み込み中…