Methanesulfonic Acid → HCID 59584818, 화합물

HRID 1253402

반응식

HRID 1253402 반응식
CS(O)(=O)=O.[NH2:6][CH:7]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:8][OH:9].[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][CH2:8][CH:7]([NH2:6])[CH2:10][CH2:11][CH2:12][CH3:13])(=[O:22])[CH2:20][CH2:19][S:18][S:17][CH2:16][CH2:15][C:14]([O:9][CH2:8][CH:7]([NH2:6])[CH2:10][CH2:11][CH2:12][CH3:13])=[O:25]

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 951163,3'-Dithiodipropionic acidHCID 249006DL-2-Amino-1-hexanol

생성물 1

HCID 59584818HCID 59584818, 화합물

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

반응 조건

온도
120 °C

실험 절차

6.1 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 7.0 g of 2-amino-1-hexanol (manufactured by Aldrich Co., Ltd.). After stifling for 10 minutes, 6.3 g of 3,3′-dithiodipropionic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, and the resulting mixture was heated to 120° C. The mixture was then stirred at 120 to 129° C. for a further 3 hours. Following completion of the reaction, the reaction mixture was cooled to room temperature and then added gradually to 100 mL of methyl isobutyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.). After stifling for 1 hour, the precipitated crystals were collected by filtration and dried at 50° C., yielding the methanesulfonate salt of di(2-aminohexyl) 3,3′-dithiodipropionate.

후처리

  1. customcompletion of the reaction
  2. temperaturethe reaction mixture was cooled to room temperature
  3. waitAfter stifling for 1 hour
  4. filtrationthe precipitated crystals were collected by filtration
  5. customdried at 50° C.

출처 및 근거

ORD 기록
ord-1477f1b097fe4093b22526e1171ef0a6
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455413B2

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