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

HRID 1650203노트

반응식

HRID 1650203 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9c6b1afd6fc84625a2065b3868b10a07
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04923882

반응 노트

불러오는 중…