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Triethylamine → N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanyl-3-(4-thiazolyl)-DL-alanine methyl ester

HRID 255626
ノート
印刷プレビュー

反応式

HRID 255626 の反応式
[CH2:1]([O:8][C:9]([NH:11][C@H:12]([C:24](O)=[O:25])[CH2:13][C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[CH:16][CH:15]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.Cl.[CH3:29][O:30][C:31](=[O:40])[CH:32]([CH2:34][C:35]1[N:36]=[CH:37][S:38][CH:39]=1)[NH2:33].P(C#N)(=O)(OCC)OCC.C(N(CC)CC)C>O1CCCC1>[CH3:29][O:30][C:31](=[O:40])[CH:32]([CH2:34][C:35]1[N:36]=[CH:37][S:38][CH:39]=1)[NH:33][C:24](=[O:25])[C@H:12]([CH2:13][C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[CH:16][CH:15]=1)[NH:11][C:9]([O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 7020250Z-1-Nal-OHHCID 217527263-(4-thiazolyl)-DL-alanine methyl ester dihydrochloride

生成物 1

HCID 53931154N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanyl-3-(4-thiazolyl)-DL-alanine methyl ester収率 61%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

2.90 g (8.30 mmole) of N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanine and 2.15 g (8.30 mmole) of 3-(4-thiazolyl)-DL-alanine methyl ester dihydrochloride were suspended in 30 ml of anhydrous tetrahydrofuran. Whilst ice cooling, 1.51 ml (9.95 mmole) of diethyl phosphorocyanidate and 3.82 ml (27.4 mmole) of triethylamine were added dropwise under a nitrogen gas stream, and the mixture was stirred overnight at room temperature. The reaction product was condensed by evaporation under reduced pressure. Ethyl acetate was added to the residue, and the mixture was washed with water and then dried over anhydrous magnesium sulfate. The dried product was condensed by evaporation under reduced pressure, and the residue was purified by silica gel column chromatography eluted with a 10:1 by volume mixture of chloroform and methanol, to yield 2.62 g (61%) of N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanyl-3-(4-thiazolyl)-DL-alanine methyl ester.

後処理

  1. customcondensed
  2. customby evaporation under reduced pressure
  3. additionEthyl acetate was added to the residue
  4. washthe mixture was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customcondensed
  7. customby evaporation under reduced pressure
  8. customthe residue was purified by silica gel column chromatography
  9. washeluted with a 10:1 by volume mixture of chloroform and methanol

出典と根拠

ORDレコード
ord-9c3f5db1418c4f6784e64ad437444329
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04698329

反応ノート

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