Nitrogen → Octanethioic acid, S-(3-(triethoxysilyl)propyl) ester

HRID 64501

反応式

HRID 64501 の反応式
N#N.[SH:3][CH2:4][CH2:5][CH2:6][Si:7]([O:14][CH2:15][CH3:16])([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10].C(N(CC)CC)C.[C:24](Cl)(=[O:32])[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]>CCCCCC>[C:24]([S:3][CH2:4][CH2:5][CH2:6][Si:7]([O:14][CH2:15][CH3:16])([O:8][CH2:9][CH3:10])[O:11][CH2:12][CH3:13])(=[O:32])[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]

参加物

6

反応物 4

HCID 947NitrogenHCID 8124Octanoyl chlorideHCID 8471TriethylamineHCID 846581-Propanethiol, 3-(triethoxysilyl)-

生成物 1

HCID 12135713Octanethioic acid, S-(3-(triethoxysilyl)propyl) ester収率 99.2%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 3-mercaptopropyltriethoxysilane (1,021 grams, 3.73 moles purchase as SILQUEST® A-1891 silane from Momentive Performance Materials, Inc.), triethylamine (433 grams), and hexane (3,000 ml). The solution was cooled in an ice bath, and octanoyl chloride (693 grams, 4.25 moles) were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent.

後処理

  1. customInto a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel
  2. temperatureThe solution was cooled in an ice bath
  3. filtrationthe mixture was filtered two times
  4. filtrationfirst through a 0.1 μm filter
  5. filtrationthrough a 0.01 μm filter
  6. filtrationfilter
  7. customto remove the salt
  8. customThe solvent was removed under vacuum
  9. distillationdistilled

出典と根拠

ORDレコード
ord-cc4ab92194bd493f9ad2faa2b80e1bab
出典データセット
uspto-grants-2016_09
特許番号
US09447262B2

関連ノート

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