Hydrochloric Acid → (S,S)-2,7-Diamino-(Z)-oct-4-ene-1,8-dioic acid dimethylester

HRID 976014노트

반응식

HRID 976014 반응식
COC1[C@@H](C(C)C)N=[C:6]([O:26]C)[C@H:7]([CH2:9]/[CH:10]=[CH:11]\[CH2:12][C@H:13]2[C:18]([O:19][CH3:20])=N[C@H](C(C)C)C(OC)=[N:14]2)[N:8]=1.Cl.CC#N.[CH3:35][OH:36].[O:37]1CCOCC1>O>[CH3:35][O:36][C:6](=[O:26])[C@@H:7]([NH2:8])[CH2:9]/[CH:10]=[CH:11]\[CH2:12][C@H:13]([NH2:14])[C:18]([O:19][CH3:20])=[O:37]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 887MethanolHCID 6342AcetonitrileHCID 312751,4-DioxaneHCID 676524241,4-Bis((2R,5S)-2,5-dihydro-3,6-dimethoxy-2-isopropyl-5-pyrazinyl)-(Z)-but-2-ene

생성물 1

HCID 86750551(S,S)-2,7-Diamino-(Z)-oct-4-ene-1,8-dioic acid dimethylester

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1,4-Bis((2R,5S)-2,5-dihydro-3,6-dimethoxy-2-isopropyl-5-pyrazinyl)-(Z)-but-2-ene (0.58 g, 1.23 mmol) was dissolved in dioxane (8 ml), and 0.25M HCl (8 ml, 2.5 mmol) was added and stirred overnight at ambient temperature. TLC(MeCN:MeOH:H2O/4:1:1). The solution was extracted with diethyl ether, and the aqueous phase was evaporated. The residue was dissolved in a small amount of water, and aqueous ammonia solution was added until a pH of 9 was reached. The aqueous phase was extracted twice with diethyl ether, and the organic phase was dried over MgSO4 and evaporated.

후처리

  1. extractionThe solution was extracted with diethyl ether
  2. customthe aqueous phase was evaporated
  3. dissolutionThe residue was dissolved in a small amount of water, and aqueous ammonia solution
  4. additionwas added until a pH of 9
  5. extractionThe aqueous phase was extracted twice with diethyl ether
  6. dry with materialthe organic phase was dried over MgSO4
  7. customevaporated

출처 및 근거

ORD 기록
ord-948eafc57b9e411fbf4c5f55e29736df
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05610141

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