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Hydrochloric Acid → N-myristoyl-D-serine sodium salt

HRID 1196070
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HRID 1196070 반응식
[NH2:1][C@@H:2]([C:5]([OH:7])=[O:6])[CH2:3][OH:4].C(N(CC)CC)C.[C:15]([O-])(=[O:29])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].S([O-])([O-])(=O)=O.Cl.[OH-].[Na+:38]>O.C(OCC)(=O)C.CO>[Na+:38].[C:15]([NH:1][C@@H:2]([C:5]([O-:7])=[O:6])[CH2:3][OH:4])(=[O:29])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 1117Sulfate IonHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 71077D-SerineHCID 4075158Myristate

생성물 1

HCID 131717352N-myristoyl-D-serine sodium salt

시약·촉매·용매

2
HCID 962Water용매HCID 21584119Ethylacetate methanol용매

실험 절차

D-serine 2.0 g (0.02 mole) and triethylamine 2.8 ml (0.02 mol) were dissolved in 60 ml of water. Myristate of 4-hydroxyphenyldimethylsufomethyl sulfate (trade name: SANCELER My-DSP, manufactured by Sanshin Kagaku Kogyo Co. Ltd.) 9.52 g (0.02 mol) was added to the solution, and the mixture was stirred for 12 hours at room temperature. The solution reacted was adjusted to pH 2 or 3 with 1N-HCl and the mixture was extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous sodium sulfate, and freed of solvent in vacuo. The residue obtained was dissolved in ethyl acetate - methanol (3:1), and the solution was adjusted to pH 11 with a 10% solution of sodium hydroxide. After observation of precipitates, the solution was concentrated under reduced pressure. The product crystallized was washed with ethyl acetate and then hexane to obtain 3.1 g of N-myristoyl-D-serine sodium salt.

후처리

  1. customThe solution reacted
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  4. customThe residue obtained
  5. customAfter observation of precipitates
  6. concentrationthe solution was concentrated under reduced pressure
  7. customThe product crystallized
  8. washwas washed with ethyl acetate

출처 및 근거

ORD 기록
ord-9ec6cd2360e64ff9a4f8cab33eea4825
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05112863

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