Methanesulfonic Acid → HCID 59584818、化合物

HRID 1253402ノート

反応式

HRID 1253402 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 59584818HCID 59584818、化合物

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

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.

後処理

  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.

出典と根拠

ORDレコード
ord-1477f1b097fe4093b22526e1171ef0a6
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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