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Methylamine → HCID 11391445、化合物

HRID 1838900
ノート
印刷プレビュー

反応式

HRID 1838900 の反応式
[CH3:1][NH2:2].IC[CH2:5][CH2:6][CH:7]([S:17][CH:18](CCCI)[CH2:19][CH2:20][C:21]([F:27])([F:26])[C:22]([F:25])([F:24])[F:23])CCC(F)(F)C(F)(F)F>O1CCCC1>[CH3:1][NH:2][CH2:5][CH2:6][CH2:7][S:17][CH2:18][CH2:19][CH2:20][C:21]([F:27])([F:26])[C:22]([F:25])([F:24])[F:23]
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 6329MethylamineHCID 865876413-Iodopropyl-4,4,5,5,5-pentafluoropentylsulfide

生成物 1

HCID 11391445HCID 11391445、化合物収率 133.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

45 g of methylamine are condensed at a bath temperature of −78° C. into a solution of 30.6 g of 3-iodopropyl-4,4,5,5,5-pentafluoropentyl sulphide in 200 ml of abs. tetrahydrofuran and the mixture is stirred at room temperature for 1.5 hours and at 60° C. for 4 hours in a pressure reactor. To open the reactor, it is allowed to cool overnight to room temperature and then to −78° C. It is then allowed to come to room temperature, excess methylamine is evaporated, the mixture is diluted with ethyl acetate, washed until neutral, dried over sodium sulphate and concentrated in vacuo, and the residue is chromatographed on silica gel using dichloromethane/methanol. 15.7 g of N-methyl-[3-(4,4,5,5,5-pentafluoro-pentylthio)propyl]amine are obtained as an oil.

後処理

  1. temperatureto cool overnight to room temperature
  2. customto −78° C
  3. customto come to room temperature
  4. customexcess methylamine is evaporated
  5. additionthe mixture is diluted with ethyl acetate
  6. washwashed until neutral,
  7. dry with materialdried over sodium sulphate
  8. concentrationconcentrated in vacuo
  9. customthe residue is chromatographed on silica gel

出典と根拠

ORDレコード
ord-3b7e9b58bee244ae8ebaf4ae893669c7
出典データセット
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06677324B1

反応ノート

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