Sodium Hydroxide → HCID 10666287, 화합물

HRID 2237338

반응식

HRID 2237338 반응식
[ClH:1].[NH2:2][CH2:3][CH2:4][S:5][S:6][CH2:7][CH2:8][NH2:9].[OH-:10].[Na+].[Cl:12][CH2:13][CH2:14][CH2:15][C:16](Cl)=[O:17]>C1COCC1>[S:5]([CH2:4][CH2:3][NH:2][C:13](=[O:10])[CH2:14][CH2:15][CH2:16][Cl:1])[S:6][CH2:7][CH2:8][NH:9][C:16](=[O:17])[CH2:15][CH2:14][CH2:13][Cl:12]

참가 물질

5

반응물 3

HCID 14798Sodium Hydroxide2회HCID 783704-Chlorobutyryl chlorideHCID 1676282-[(2-Aminoethyl)disulfanyl]ethan-1-amine hydrochloride

생성물 1

HCID 10666287HCID 10666287, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
5 °C

실험 절차

60 g of cystamine hydrochloride was solubilized in 500 mL and cooled to 5° C. The pH was raised to 10 by addition of aq. NaOH (30%). A solution of 4-chlorobutanoyl chloride (105 g) in anhydrous THF (500 mL), was added dropwise, while the pH was maintained above 7 by addition of aq. NaOH (30%). After completion of the addition and stabilization of pH at 7, the mixture mixed for 3 days. The aqueous layer was extracted with 3×500 mL dichloromethane, combined with THF layer and dried over Na2SO4. After drying under vacuum, 41 g of a white powder were collected. Analyses were in accordance with the expected structure.

후처리

  1. additionAfter completion of the addition and stabilization of pH at 7
  2. additionthe mixture mixed for 3 days
  3. extractionThe aqueous layer was extracted with 3×500 mL dichloromethane
  4. dry with materialdried over Na2SO4
  5. dry with materialAfter drying under vacuum, 41 g of a white powder
  6. customwere collected

출처 및 근거

ORD 기록
ord-0c79e47db59f4b84a45a00062d668bae
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07717964B2

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