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Toluene → 4-(2-Pyridylmethyl)-2,2,6,6-tetramethyl-1-oxa-4-aza-2,6-disilacyclohexane

HRID 27875
ノート
印刷プレビュー

反応式

HRID 27875 の反応式
I[CH2:2][Si:3]([CH3:11])([CH3:10])[O:4][Si:5]([CH2:8]I)([CH3:7])[CH3:6].[NH2:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1.C1(C)C=CC=CC=1>O>[N:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][N:12]1[CH2:8][Si:5]([CH3:6])([CH3:7])[O:4][Si:3]([CH3:11])([CH3:10])[CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1140TolueneHCID 195092-PyridinemethanamineHCID 2566811,3-Bis(iodomethyl)-1,1,3,3-tetramethyldisiloxane

生成物 1

HCID 233402924-(2-Pyridylmethyl)-2,2,6,6-tetramethyl-1-oxa-4-aza-2,6-disilacyclohexane

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 41.4 g. (0.1 mole) of 1,3-bis-iodomethyl-1,1,3,3-tetramethyl-disiloxane there is added dropwise with stirring 32.4 g. (0.3 mole) of 2-aminomethyl-pyridine while maintaining the temperature at 20° C. Stirring is continued at room temperature for 24 hours. The now heterogeneous mixture is combined with approximately 0.5 l. of toluene followed by approximately 0.5 l. of water. The equilibrated aqueous phase is then extracted with two 100 ml. portions of toluene. The combined organic phase is then washed twice with approximately 100 ml. of water to give 4-(2-pyridylmethyl)-2,2,6,6-tetramethyl-1-oxa-4-aza-2,6-disilacyclohexane as the crude free base.

後処理

  1. stirringStirring
  2. extractionThe equilibrated aqueous phase is then extracted with two 100 ml
  3. washThe combined organic phase is then washed twice with approximately 100 ml

出典と根拠

ORDレコード
ord-88eb27fe145143528c64dd0096180b8c
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04224317

反応ノート

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