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Silane, trichlorodecyl- → Dichloro(didecyl)silane

HRID 1772569
ノート
印刷プレビュー

反応式

HRID 1772569 の反応式
[CH2:1]([Si:11]([Cl:14])([Cl:13])Cl)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[CH2:15]([Mg]Br)[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]>O1CCCC1>[Cl:14][Si:11]([Cl:13])([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 83764Silane, trichlorodecyl-HCID 178418384HCID 178418384、化合物

生成物 1

HCID 21889368Dichloro(didecyl)silane収率 65%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Tetrahydrofuran (82 mL) and n-decyltrichlorosilane (Tokyo Chemical Industry Co., Ltd., 14.5 g, 52.6 mmol) were placed in a 500 mL four-necked flask in a nitrogen atmosphere, and cooled to 0° C. n-decyl magnesium bromide (Sigma-Aldrich Co. LLC., 1.0 M, 58 ml) was added dropwise, and the mixture was agitated for 1 hour at 10° C. or less. The temperature was raised gradually to room temperature over the course of about 1 hour, and the mixture was left standing overnight. The precipitated salt was filtered out, the tetrahydrofuran was removed by concentration under reduced pressure, and distillation under reduced pressure was performed to obtain the target dichlorodi-n-decylsilane (Compound E21) (150° C./0.1-0.2 Torr, 13.1 g, yield 65%).

後処理

  1. additionwas added dropwise
  2. waitthe mixture was left
  3. waitstanding overnight
  4. filtrationThe precipitated salt was filtered out
  5. customthe tetrahydrofuran was removed by concentration under reduced pressure, and distillation under reduced pressure

出典と根拠

ORDレコード
ord-b706dc5cd6ea485c9a386bb738c41dbf
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09249257B2

反応ノート

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