Phenylphosphonic dichloride → 1-phenyl-2-(3-methylphenyl)-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide

HRID 2058889

反応式

HRID 2058889 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:5]=[CH:6][CH:7]=1.[C:16]1([P:22](Cl)(Cl)=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>>[C:16]1([P:22]2(=[O:23])[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[CH2:9][N:8]2[C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[CH:3]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

3

反応物 2

HCID 69990Phenylphosphonic dichloride2 回HCID 222281N-(3-Methylphenyl)benzenemethanamine

生成物 1

HCID 130374901-phenyl-2-(3-methylphenyl)-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide

実験手順

The procedure of Example 1 was employed utilizing N-3-methylphenyl-N-benzylamine and phenyl phosphonic dichloride. The reaction of the dilithio compound and the phenyl phosphonic dichloride was conducted at 0° C. The crude product produced as a result of the chromatographic separation was crystallized from diethyl ether then recrystallized from carbon tetrachloride to yield 1-phenyl-2-(3-methylphenyl)-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide as a yellow solid. A second crop was obtained to give a total yield of 1.2 g (12% yield) of 1-phenyl-2-(3-methylphenyl)-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide having a melting point of 190°-192° C. and the following analysis:

後処理

  1. customwas conducted at 0° C
  2. customThe crude product produced as
  3. customa result of the chromatographic separation
  4. customwas crystallized from diethyl ether
  5. customthen recrystallized from carbon tetrachloride

出典と根拠

ORDレコード
ord-bd26b2908b814b9fa899bb9bc2019f9b
出典データセット
uspto-grants-1982_03
特許番号
US04319913

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