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

HRID 976014ノート

反応式

HRID 976014 の反応式
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]

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-948eafc57b9e411fbf4c5f55e29736df
出典データセット
uspto-grants-1997_03
特許番号
US05610141

反応ノート

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