2-Amino-1-(3-methylphenyl)ethan-1-ol → 1-{[2-Hydroxy-2-(3-methylphenyl)ethyl]amino}-1-methylthio-2-nitroethene

HRID 236258ノート

反応式

HRID 236258 の反応式
[CH3:1][S:2]([C:4](SC)=[CH:5][N+:6]([O-:8])=[O:7])=O.[CH3:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH:18]([OH:21])[CH2:19][NH2:20])[CH:13]=1>C(O)C>[OH:21][CH:18]([C:14]1[CH:15]=[CH:16][CH:17]=[C:12]([CH3:11])[CH:13]=1)[CH2:19][NH:20][C:4]([S:2][CH3:1])=[CH:5][N+:6]([O-:8])=[O:7]

参加物

4

反応物 2

HCID 134825112-Amino-1-(3-methylphenyl)ethan-1-olHCID 544870941-Nitro2-methylthio-2-methylsulphinylethylene

生成物 1

HCID 678972801-{[2-Hydroxy-2-(3-methylphenyl)ethyl]amino}-1-methylthio-2-nitroethene収率 50.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In 50 ml of anhydrous ethanol was suspended 9.3 g of 1-methylsulfinyl-1-methylthio-2-nitroethene, and the resulting suspension was stirred. A solution of 9.3 g of DL-[2-hydroxy-2-(3-methylphenyl)ethyl]amine in 5 ml of ethanol was added thereto dropwise at -10° C. to 0° C. over a period of 30 minutes in a nitrogen atmosphere. After the addition, the resulting mixture was stirred at the same temperature for 1.5 hours, and the crystals deposited were collected by filtration, washed with 10 ml of ethanol, and then dried to obtain 7.0 g (yield 50.8%) of 1-{[2-hydroxy-2-(3-methylphenyl)ethyl]amino}-1-methylthio-2-nitroethene having a melting point of 99°-101° C.

後処理

  1. additionAfter the addition
  2. stirringthe resulting mixture was stirred at the same temperature for 1.5 hours
  3. filtrationthe crystals deposited were collected by filtration
  4. washwashed with 10 ml of ethanol
  5. customdried

出典と根拠

ORDレコード
ord-bcf45762910841ee8260c803f8347cc4
出典データセット
uspto-grants-1987_02
特許番号
US04643849

反応ノート

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