N-(1,1-Dimethylethyl)benzenemethanamine → 1-isopropyl-2-t-butyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide

HRID 2058910ノート

反応式

HRID 2058910 の反応式
[C:1]([NH:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)([CH3:4])([CH3:3])[CH3:2].[CH:13]([P:16](Cl)(Cl)=[O:17])([CH3:15])[CH3:14]>>[CH:13]([P:16]1(=[O:17])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][N:5]1[C:1]([CH3:4])([CH3:2])[CH3:3])([CH3:15])[CH3:14]

参加物

3

反応物 2

HCID 76908N-(1,1-Dimethylethyl)benzenemethanamineHCID 2793751Isopropylphosphonic dichloride2 回

生成物 1

HCID 130375101-isopropyl-2-t-butyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide収率 39%

実験手順

The procedure of Example 30 was employed utilizing N-t-butyl-N-benzylamine and isopropyl phosphonic dichloride. The reaction of the dilithio compound and the isopropyl phosphonic dichloride was conducted at -70° C. The crude product produced as a result of the chromatographic separation was distilled at 130° C. and 0.1 mm to yield a colorless oil. The colorless oil was slurried in petroleum ether to yield 1-isopropyl-2-t-butyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide (5.8 g, 39% yield) having a melting point of 67°-70° C. and the following analysis:

後処理

  1. customwas conducted at -70° C
  2. customThe crude product produced as
  3. customa result of the chromatographic separation
  4. distillationwas distilled at 130° C.
  5. custom0.1 mm to yield a colorless oil

出典と根拠

ORDレコード
ord-388583c4b5634feeb00f4a7b670ffba2
出典データセット
uspto-grants-1982_03
特許番号
US04319913

反応ノート

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