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3-Nitrophenylboronic Acid → HCID 178442840、化合物

HRID 343992
ノート
印刷プレビュー

反応式

HRID 343992 の反応式
[NH2:1][NH:2][C:3]([NH:5][NH2:6])=[S:4].[CH2:7]([C:22]1[CH:23]=[C:24]([CH:32]=[CH:33][CH:34]=1)[O:25][CH:26]([CH2:30][CH3:31])[C:27](O)=O)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21].[N+](C1C=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:27]1[CH:26]([O:25][C:24]1[CH:32]=[CH:33][CH:34]=[C:22]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH:23]=1)[CH2:30][CH3:31]
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 16773-Nitrophenylboronic AcidHCID 85701Butanoic acid, 2-(3-pentadecylphenoxy)-HCID 2724189Thiocarbohydrazide

生成物 1

HCID 178442840HCID 178442840、化合物収率 62.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a mixture of 2.65 g (25 mmol) of thiocarbohydrazide and 9.77 g (25 mmol) of 2-(3-pentadecylphenoxy)butanoic acid in 30 mL of toluene was added 0.42 g (2.5 mmol) of 3-nitrobenzene boronic acid was heated at reflux for 24 hr. The reaction was cooled and the reaction was allowed to settle. The supernatant liquid was decanted. To the residual solid was added 20 mL of acetonitrile. The mixture was stirred for 15 minutes. The solid was collected, rinsed with 5 mL of cold acetonitrile and dried in vacuo to afford 7.20 g (60.4%) of the desired product as a white solid. Analytical data are consistent with the assigned structure.

後処理

  1. temperaturewas 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 20 mL of acetonitrile
  6. customThe solid was collected
  7. washrinsed with 5 mL of cold acetonitrile
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-fd15fe57b54949099606cbe393af5899
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05864042

反応ノート

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