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p-Toluenesulfonic acid → HCID 131720843、化合物

HRID 2395125
ノート
印刷プレビュー

反応式

HRID 2395125 の反応式
CN1CCOCC1.[NH:8]([C:21]([O:23][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:22])[C@H:9]([C:18]([OH:20])=O)[CH2:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14].O.[NH2:32][C@H:33]([C:37]([O:39][CH2:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)=[O:38])[CH:34]([CH3:36])[CH3:35].S(O)(C1C=CC(C)=CC=1)(=O)=O>CN(C=O)C>[NH:8]([C:21]([O:23][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:22])[C@H:9]([C:18]([NH:32][C@H:33]([C:37]([O:39][CH2:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)=[O:38])[CH:34]([CH3:36])[CH3:35])=[O:20])[CH2:10][C:11](=[O:17])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16]
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 6101p-Toluenesulfonic acidHCID 79724-MethylmorpholineHCID 6950584benzyl (2S)-2-amino-3-methylbutanoateHCID 74892349Z-Asp(OtBu)-OH·H2O

生成物 1

HCID 131720843HCID 131720843、化合物収率 85.4%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

15.83 g of 1-benzotriazol-1-yl-N,N,N',N'-tetramethyluronium hexafluorophosphate and 9 ml of N-methylmorpholine were added to a solution of 13.65 g of Z-Asp(OBut)-OH.H2O and 15.9 g of Val-OBzl.TosOH in 250 ml of DMF. After stirring for 2 hours the reaction mixture was evaporated in a vacuum and the residue was partitioned between ethyl acetate and water. The organic phase was washed with 5% KHSO4 10% K2SO4 solution, water, saturated NaHCO3 solution, water and saturated NaCl solution, dried over Na2SO4, filtered and evaporated. The residue was crystallized from diethyl ether/hexane and there were obtained 17.5 g of Z-Asp(OBut)-Val-OBzl of m.p. 99°; [α]D20 -27.7° (c=1, MeOH).

後処理

  1. customwas evaporated in a vacuum
  2. customthe residue was partitioned between ethyl acetate and water
  3. washThe organic phase was washed with 5% KHSO4 10% K2SO4 solution, water, saturated NaHCO3 solution, water and saturated NaCl solution
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was crystallized from diethyl ether/hexane

出典と根拠

ORDレコード
ord-14ee0af7adfd45e88690ae6dbd3d698a
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05811389

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート