Tributylamine → Bu3SnBr Bu2SnBr2

HRID 1980466

反応式

HRID 1980466 の反応式
[CH2:1]([Sn:5]([Br:14])([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[CH2:15]([Sn:19]([Br:25])([Br:24])[CH2:20][CH2:21][CH2:22][CH3:23])[CH2:16][CH2:17][CH3:18].C(N(CCCC)CCCC)CCC.[Sn].C(Br)CCC>>[Sn:5]([Br:14])([CH2:6][CH2:7][CH2:8][CH3:9])([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:1][CH2:2][CH2:3][CH3:4].[Sn:19]([CH2:20][CH2:21][CH2:22][CH3:23])([CH2:15][CH2:16][CH2:17][CH3:18])([Br:25])[Br:24]

参加物

6

反応物 5

HCID 7622TributylamineHCID 8002Butyl bromideHCID 93569DibromodibutylstannaneHCID 305767Tributyltin bromideHCID 5352426Tin atom

生成物 1

HCID 131713428Bu3SnBr Bu2SnBr2

実験手順

Crude tributyltin bromide (Bu3SnBr) containing up to 28% dibutyltin dibromide (Bu2SnBr2), and halogenotin by-product were prepared in a series of experiments, A-G. These involved heating tributylamine (Bu3N) with excess elemental tin and adding butyl bromide (BuBr) at a rate such that the reaction temperature of 130°-140°. was maintained. When this addition was complete, the reaction mass was maintained at 130°-140° for several hours more. Excess BuBr was then removed by distillation. After cooling to about 60°-80° the reaction liquor was decanted from the unreacted tin and extracted with 3 volumes of hydrocarbon spirits (b.p 145°-160°). The extracts were combined and the hydrocarbon distilled off leaving the crude Bu3SnBr-Bu2SnBr2 mixture. The halogenotin complex by-product remaining after the extraction was heated under vacuum to remove any residual hydrocarbon extractment and the product stored in plastic containers. The amounts of materials used and the products obtained are shown in table III.

後処理

  1. customwere prepared in a series of experiments, A-G
  2. temperaturewas maintained
  3. additionWhen this addition
  4. temperaturethe reaction mass was maintained at 130°-140° for several hours more
  5. customExcess BuBr was then removed by distillation
  6. temperatureAfter cooling to about 60°-80° the reaction liquor
  7. customwas decanted from the unreacted tin
  8. extractionextracted with 3 volumes of hydrocarbon spirits (b.p 145°-160°)
  9. distillationthe hydrocarbon distilled off

出典と根拠

ORDレコード
ord-fcd7374b484547bfad23ee2dd8338740
出典データセット
uspto-grants-1985_04
特許番号
US04510095

関連ノート

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