Methylamine → Methyl-(7,7,8,8,9,9,10,10,10-nonafluorodecyl)amine

HRID 1837260ノート

反応式

HRID 1837260 の反応式
[CH3:1][NH2:2].[F:3][C:4]([F:32])([C:22]([F:31])([F:30])[C:23]([F:29])([F:28])[C:24]([F:27])([F:26])[F:25])[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10]C1C=C(C)C=CC=1S([O-])(=O)=O>O1CCCC1>[CH3:1][NH:2][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][C:4]([F:32])([F:3])[C:22]([F:31])([F:30])[C:23]([F:29])([F:28])[C:24]([F:27])([F:26])[F:25]

参加物

4

反応物 2

HCID 6329Methylamine2 回HCID 234970787,7,8,8,9,9,10,10,10-Nonafluoro-decyltosylate

生成物 1

HCID 12095891Methyl-(7,7,8,8,9,9,10,10,10-nonafluorodecyl)amine収率 96%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4.12 g of methylamine is condensed in a solution of 3.89 g of 7,7,8,8,9,9,10,10,10-nonafluoro-decyltosylate in 10 ml of absolute tetrahydrofuran at −20° C., and it is stirred overnight in a pressure vessel at room temperature. After the pressure vessel was opened at −20° C., it is allowed to come to room temperature to allow excess methylamine to evaporate off. The reaction solution is taken up in dichloromethane, washed with water, dried on magnesium sulfate and concentrated by evaporation in a vacuum. 2.63 g of methyl-(7,7,8,8,9,9,10,10,10-nonafluoro-decyl)-amine is obtained as a crude product.

後処理

  1. customwas opened at −20° C.
  2. customto come to room temperature
  3. customto evaporate off
  4. washwashed with water
  5. customdried on magnesium sulfate
  6. concentrationconcentrated by evaporation in a vacuum

出典と根拠

ORDレコード
ord-e033aaf5e2004e9d91f2e58b2a5f5fba
出典データセット
uspto-grants-2004_08
特許番号
US06780855B2

反応ノート

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