Methanamine, N-methyl-, titanium(4+) salt (4:1) → HCID 178445874、化合物

HRID 441780ノート

反応式

HRID 441780 の反応式
[CH2:1]([Li])[C:2]([CH3:5])([CH3:4])[CH3:3].[CH3:7][N-:8][CH3:9].[CH3:10][N-:11][CH3:12].C[N-]C.C[N-]C.[Ti+4:19]>CCCCC>[CH3:7][N-:8][CH3:9].[CH3:10][N-:11][CH3:12].[CH2:1]([Ti+2:19][CH2:1][C:2]([CH3:5])([CH3:4])[CH3:3])[C:2]([CH3:5])([CH3:4])[CH3:3]

参加物

4

反応物 2

HCID 123185Methanamine, N-methyl-, titanium(4+) salt (4:1)HCID 178506860HCID 178506860、化合物

生成物 1

HCID 178445874HCID 178445874、化合物収率 86.4%

試薬・触媒・溶媒 1

HCID 8003Pentane溶媒2 回

実験手順

A solution of 4.87 g of neopentyllithium in pentane was added to a solution of 7.0 g of titanium tetrakis(dimethylamide) in pentane with stirring. Lithium dimethylamide precipitated rapidly. The total amount of pentane in the reaction mixture was about 50-100 ml. After being stirred for one hour the mixture was filtered, and pentane was evaporated from the filtrate to give 7.5 g (86%) of dineopentyltitanium bis(dimethylamide) as an air-sensitive yellow oil. Nmr C6D6 : δ (NMe) 3.23, δ (CMe3) 1.05 ppm downfield from tetramethylsilane.

後処理

  1. customLithium dimethylamide precipitated rapidly
  2. stirringAfter being stirred for one hour the mixture
  3. filtrationwas filtered
  4. custompentane was evaporated from the filtrate

出典と根拠

ORDレコード
ord-ecfc3bb4034f4f9a85184e67ee71ac0a
出典データセット
uspto-grants-1977_08
特許番号
US04042610

反応ノート

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