Toluene → 4-(2-Thienylmethyl)-2,2,6,6-tetra-methyl-1-oxa-4-aza-2,6-disilacyclohexane

HRID 27876

反応式

HRID 27876 の反応式
[C:1]1([CH2:6][NH2:7])[S:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.Cl[CH2:16][Si:17]([CH3:25])([CH3:24])[O:18][Si:19]([CH2:22]Cl)([CH3:21])[CH3:20].C1(C)C=CC=CC=1>O>[S:5]1[CH:4]=[CH:3][CH:2]=[C:1]1[CH2:6][N:7]1[CH2:20][Si:19]([CH3:22])([CH3:21])[O:18][Si:17]([CH3:25])([CH3:24])[CH2:16]1

参加物

6

反応物 4

HCID 1140TolueneHCID 8471TriethylamineHCID 34005(2-Thienylmethyl)amineHCID 753851,3-Bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane

生成物 1

HCID 233402954-(2-Thienylmethyl)-2,2,6,6-tetra-methyl-1-oxa-4-aza-2,6-disilacyclohexane

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

To a solution containing 22.6 g. (0.2 mole) of 2-thenylamine, 44.4 g. (0.44 mole) of triethylamine and 50.0 g. of acetonitrile dried over molecular sieves there is added 46.2 g. (0.2 mole) of 1,3-bis-chloromethyl-1,1,3,3-tetramethyl-disiloxane. The resulting homogenized solution is allowed to stand for 3 days and then heated in a bath at 90° C. for 36 hours. After cooling the mixture is then equiliberated between toluene and water, the organic phase is then washed with two more portions of water and concentrated to give 61.5 g. of a crude oil. Vacuum distillation through a Vigreux column gives 4-(2-thienylmethyl)-2,2,6,6-tetra-methyl-1-oxa-4-aza-2,6-disilacyclohexane; b.p. 78° to 80° C. at 0.1 to 0.11 mm.

後処理

  1. additionTo a solution containing 22.6 g
  2. dry with materialof acetonitrile dried over molecular sieves there
  3. additionis added 46.2 g
  4. temperatureAfter cooling the mixture
  5. washthe organic phase is then washed with two more portions of water
  6. concentrationconcentrated
  7. customto give 61.5 g
  8. distillationVacuum distillation through a Vigreux column

出典と根拠

ORDレコード
ord-daa0191ef4ad4921942a85e01f0b9bb3
出典データセット
uspto-grants-1980_09
特許番号
US04224317

関連ノート

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