Methanesulfonic Acid → Di(6-aminohexyl) 3,3'-dithiodipropionate

HRID 1253399

반응식

HRID 1253399 반응식
CS(O)(=O)=O.[NH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13].[C:14]([OH:25])(=O)[CH2:15][CH2:16][S:17][S:18][CH2:19][CH2:20][C:21]([OH:23])=[O:22]>C(C(C)=O)C(C)C>[C:21]([O:23][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][NH2:6])(=[O:22])[CH2:20][CH2:19][S:18][S:17][CH2:16][CH2:15][C:14]([O:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][NH2:6])=[O:25]

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 199606-Amino-1-hexanolHCID 951163,3'-Dithiodipropionic acid

생성물 1

HCID 59584809Di(6-aminohexyl) 3,3'-dithiodipropionate

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

반응 조건

온도
120 °C

실험 절차

2.0 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 6-amino-1-hexanol (manufactured by Tokyo Chemical Industry Co., Ltd.). After stirring for 10 minutes, 2.1 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 3 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 vacuum filtration and washed with acetone, yielding the methanesulfonate salt of di(6-aminohexyl) 3,3′-dithiodipropionate.

후처리

  1. stirringstirred at 110° C. for 3 hours
  2. customcompletion of the reaction
  3. temperaturethe reaction mixture was cooled to room temperature
  4. stirringAfter stirring for 2 hours
  5. filtrationthe precipitated crystals were collected by vacuum filtration
  6. washwashed with acetone

출처 및 근거

ORD 기록
ord-5032cbba7aaf45d4a4653b80204863c5
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455413B2

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