Methanesulfonic Acid → di[6-(N,N-diethyl)aminohexyl]3,3'-dithiodipropionate

HRID 1253400ノート

反応式

HRID 1253400 の反応式
CS(O)(=O)=O.[CH2:6]([N:8]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][OH:17])[CH2:9][CH3:10])[CH3:7].[C:18]([OH:29])(=[O:28])[CH2:19][CH2:20][S:21][S:22][CH2:23][CH2:24][C:25]([OH:27])=O>C(C(C)=O)C(C)C>[CH2:9]([N:8]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][O:17][C:25](=[O:27])[CH2:24][CH2:23][S:22][S:21][CH2:20][CH2:19][C:18]([O:29][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][N:8]([CH2:9][CH3:10])[CH2:6][CH3:7])=[O:28])[CH2:6][CH3:7])[CH3:10]

参加物

5

反応物 3

HCID 6395Methanesulfonic AcidHCID 951163,3'-Dithiodipropionic acidHCID 2450546-(Diethylamino)-1-hexanol

生成物 1

HCID 59584812di[6-(N,N-diethyl)aminohexyl]3,3'-dithiodipropionate

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

反応条件

温度
120 °C

実験手順

1.3 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 2.3 g of the obtained 6-(N,N-diethyl)amino-1-hexanol. After stifling for 10 minutes, 1.4 g of 3,3′-dithiodipropionic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, and the resulting mixture was heated to 120° C. and then stirred at 110° C. for 4 hours. Following completion of the reaction, the reaction mixture was cooled to room temperature and then added gradually to 50 mL of methyl isobutyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.). After stirring for 2 hours, the precipitated crystals were collected by filtration and washed with acetone, yielding the methanesulfonate salt of di[6-(N,N-diethyl)aminohexyl]3,3′-dithiodipropionate.

後処理

  1. customcompletion of the reaction
  2. temperaturethe reaction mixture was cooled to room temperature
  3. stirringAfter stirring for 2 hours
  4. filtrationthe precipitated crystals were collected by filtration
  5. washwashed with acetone

出典と根拠

ORDレコード
ord-8d6007077784428b8f31c7e3d6b9d121
出典データセット
uspto-grants-2013_06
特許番号
US08455413B2

反応ノート

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