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Water → 2-(4-Cyanophenylamino)-2-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]thioacetamide

HRID 2089679
ノート
印刷プレビュー

反応式

HRID 2089679 の反応式
[C:1]([CH:3]([NH:17][C:18]1[CH:25]=[CH:24][C:21]([C:22]#[N:23])=[CH:20][CH:19]=1)[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[C:6]([O:12][CH2:13][CH2:14][OH:15])[C:5]=1[F:16])#[N:2].[NH4+]=[S:27].O>O1CCCC1.CO>[C:22]([C:21]1[CH:20]=[CH:19][C:18]([NH:17][CH:3]([C:4]2[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[C:6]([O:12][CH2:13][CH2:14][OH:15])[C:5]=2[F:16])[C:1]([NH2:2])=[S:27])=[CH:25][CH:24]=1)#[N:23]
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 2

HCID 962WaterHCID 682128854-({Cyano[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}amino)benzonitrile

生成物 1

HCID 866774072-(4-Cyanophenylamino)-2-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]thioacetamide収率 61.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

The crude product of 4-({cyano[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}amino)benzonitrile (2.77 g) obtained in Example 30 was dissolved in tetrahydrofuran (4.26 mL) and methanol (4.26 mL), and 20% aqueous ammonium sulfide solution (8.54 mL, 25 mmol) was added dropwise thereto at room temperature, and the resulting mixture was stirred at the same temperature. After completion of the reaction, water (4.26 mL) was added dropwise to the reaction mixture, and the resulting mixture was stirred at the same temperature for 0.5 hours. The precipitated solid was filtered. The filtrate obtained was sequentially washed with water and tert-butyl methyl ether, and dried to obtain the captioned compound (1.87 g) as a pale yellow solid.

後処理

  1. additionwas added dropwise to the reaction mixture
  2. stirringthe resulting mixture was stirred at the same temperature for 0.5 hours
  3. filtrationThe precipitated solid was filtered
  4. customThe filtrate obtained
  5. washwas sequentially washed with water and tert-butyl methyl ether
  6. customdried

出典と根拠

ORDレコード
ord-0ea6bf27ddda4af9944ffb0c126e0f60
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436009B2

反応ノート

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