Pyrrolidine → Bis(pyrrolidino)silacyclobutane

HRID 519417

反応式

HRID 519417 の反応式
Cl[Si:2]1(Cl)[CH2:5][CH2:4][CH2:3]1.[NH:7]1[CH2:11][CH2:10][CH2:9][CH2:8]1>>[N:7]1([Si:2]2([N:7]3[CH2:11][CH2:10][CH2:9][CH2:8]3)[CH2:5][CH2:4][CH2:3]2)[CH2:11][CH2:10][CH2:9][CH2:8]1

参加物

3

反応物 2

HCID 31268Pyrrolidine2 回HCID 753731,1-Dichlorosilacyclobutane2 回

生成物 1

HCID 58385700Bis(pyrrolidino)silacyclobutane収率 34%

実験手順

Bis(pyrrolidino)silacyclobutane was synthesized by reacting 1,1-dichlorosilacyclobutane with an excess amount of pyrrolidine (Equation 3). To do so, 23.7 ml (0.200 mol) 1,1-dichlorosilacyclobutane was added to 100.0 ml (1.20 mol) pyrrolidine in 1 L hexanes at −10° C. After bodying for two day at the room temperature, the reaction slurry was filtered to remove pyrrolidine hydrochloride salt. The filtrant was vacuum dried to give a liquid crude product which was then vacuum distilled. 15.4 g Product was isolated at 99.7% purity in 34% yield at 51° C. under 1 torr pressure. The structure of the product analyzed with 1H, 13C and 29Si NMR, FT-IR and GC-MS was in consistence with bis(pyrrolidino)silacyclobutane.

後処理

  1. filtrationthe reaction slurry was filtered
  2. customto remove pyrrolidine hydrochloride salt
  3. customdried
  4. customto give a liquid crude product which
  5. distillationvacuum distilled

出典と根拠

ORDレコード
ord-814981cf98f64db587b0d93590a00317
出典データセット
uspto-grants-2015_08
特許番号
US09117664B2

関連ノート

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