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Methyl iodide → HCID 12017704、化合物

HRID 1279611
ノート
印刷プレビュー

反応式

HRID 1279611 の反応式
[CH:1]([N:4]([S:27]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)(=[O:29])=[O:28])[C:5]1[CH:10]=[CH:9][C:8]([C:11]([F:14])([F:13])[F:12])=[CH:7][C:6]=1[NH:15][CH2:16][C:17]1[CH:26]=[CH:25][C:20]([C:21]([O:23][CH3:24])=[O:22])=[CH:19][CH:18]=1)([CH3:3])[CH3:2].[C:36]1(S(NC2C=CC(C(F)(F)F)=CC=2NCC2C=CC(C(OC)=O)=CC=2)(=O)=O)C=CC=CC=1.[H-].[Na+].CI>CN(C=O)C>[CH3:36][N:15]([CH2:16][C:17]1[CH:26]=[CH:25][C:20]([C:21]([O:23][CH3:24])=[O:22])=[CH:19][CH:18]=1)[C:6]1[CH:7]=[C:8]([C:11]([F:14])([F:13])[F:12])[CH:9]=[CH:10][C:5]=1[N:4]([S:27]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)(=[O:29])=[O:28])[CH:1]([CH3:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 22671955HCID 22671955、化合物HCID 22672017HCID 22672017、化合物

生成物 1

HCID 12017704HCID 12017704、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

Methyl 4-[2-(N-Isopropyl-phenylsulfonylamino)-5-trifluoromethylphenylaminomethyl]benzoate (200 mg) prepared by the same procedure as Example 17 by using methyl 4-(2-phenylsulfonylamino-5-trifluoromethylphenylaminomethyl)benzoate (prepared in Example 27.) was dissolved in DMF (5 ml). Sodium hydride (64 mg) and methyl iodide (200 μl) were added thereto. The mixture was stirred for 24 hours at 60° C. The reaction mixture was extracted with H2O-AcOEt, washed, dried over, filtered and concentrated under the reduced pressure. The residue was purified on silica gel column chromatography (hexane:AcOEt=5:1) to give the title compound (105 mg) having the following physical data.

後処理

  1. extractionThe reaction mixture was extracted with H2O-AcOEt
  2. washwashed
  3. customdried over,
  4. filtrationfiltered
  5. concentrationconcentrated under the reduced pressure
  6. customThe residue was purified on silica gel column chromatography (hexane:AcOEt=5:1)

出典と根拠

ORDレコード
ord-6112bb6ee0894c479cf9c48bf58db621
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06448290B1

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート