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

HRID 1253400

반응식

HRID 1253400 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8d6007077784428b8f31c7e3d6b9d121
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455413B2

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