N-Allyl-1,1,1-trimethyl-N-(trimethylsilyl)silylamine → N-trimethylsilyl-2-chloro-2-methy-1-aza-2-silacyclopentane

HRID 2382227ノート

反応式

HRID 2382227 の反応式
C[Si:2]([CH3:12])([CH3:11])[N:3]([CH2:8][CH:9]=C)[Si:4]([CH3:7])([CH3:6])[CH3:5].[Cl:13]C([SiH3])Cl>C1(C)C(C)=CC=CC=1>[CH3:7][Si:4]([CH3:5])([CH3:6])[N:3]1[CH2:8][CH2:9][CH2:12][Si:2]1([Cl:13])[CH3:11]

参加物

4

反応物 2

HCID 82125N-Allyl-1,1,1-trimethyl-N-(trimethylsilyl)silylamineHCID 57353436(Dichloromethyl)silane

生成物 1

HCID 67301002N-trimethylsilyl-2-chloro-2-methy-1-aza-2-silacyclopentane

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
65 °C

実験手順

N-trimethylsilyl-2-chloro-2-methy-1-aza-2-silacyclopentane (cyclic APMCS, which may be referred to as c-APMCS) was prepared as follows. To a 300 mL nitrogen purged bottle equipped with stir bar was added 20.1 g (0.1 mol) of N,N-bis(trimethylsilyl)allyl amine, 11.5 g (0.1 mol) of dichloromethylsilane, and 0.81 mL of 2.4 wt % Karsted's Catalyst in xylene. The solution was stirred for 72 hrs, then heated at 65° C. for 2 hrs, and heated at 100° C. for a further 3 days. The product was distilled at 85-90° C. at 25 mm Hg. GC/MS confirmed structure. Proton NMR was also used to determine structure.

後処理

  1. customTo a 300 mL nitrogen purged bottle equipped
  2. stirringThe solution was stirred for 72 hrs
  3. temperatureheated at 100° C. for a further 3 days
  4. distillationThe product was distilled at 85-90° C. at 25 mm Hg

出典と根拠

ORDレコード
ord-7b068095cd93427aadd57b2c0f15b16d
出典データセット
uspto-grants-2012_09
特許番号
US08258332B2

反応ノート

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