Chloromethyl Methyl Ether → N-methoxymethyl-N'-t-butyl-N,N'-dibenzoylhydrazine

HRID 21630

반응식

HRID 21630 반응식
[C:1]([N:5]([C:15](=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[NH:6][C:7](=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:23][O:24][CH2:25]Cl>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH3:23][O:24][CH2:25][N:6]([C:7](=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[N:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[C:15](=[O:22])[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

참가 물질

5

반응물 2

HCID 7864Chloromethyl Methyl EtherHCID 863071,2-Dibenzoyl-1-(tert-butyl)hydrazine

생성물 1

HCID 15294609N-methoxymethyl-N'-t-butyl-N,N'-dibenzoylhydrazine

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 1140Toluene용매

실험 절차

N'-t-butyl-N,N'-dibenzoylhydrazine (2 g, 0.007M) was stirred at room temperature in a two phase system of toluene-50% sodium hydroxide with 100 mg of phase transfer catalyst (tetra-n-butylammonium hydrogen sulfate). Methoxymethyl chloride (1.2 g, 0.015M) was added dropwise and the mixture was stirred 3 hours. The layers were separated and the toluene layer was washed several times with water (until the water washes were neutral). The toluene solution was dried over anhydrous magnesium sulfate and the toluene removed under vacuum to afford N-methoxymethyl-N'-t-butyl-N,N'-dibenzoylhydrazine as a thick oil.

후처리

  1. customThe layers were separated
  2. washthe toluene layer was washed several times with water (until the water washes
  3. dry with materialThe toluene solution was dried over anhydrous magnesium sulfate
  4. customthe toluene removed under vacuum

출처 및 근거

ORD 기록
ord-7d2cb3f08be145dbb405d7662fdadc8f
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424333

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