Trifluoroacetic acid → HCID 178427526、化合物

HRID 247515ノート

反応式

HRID 247515 の反応式
[NH:1]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C@@H:2]([C:7]([OH:9])=O)[CH2:3][CH:4]([CH3:6])[CH3:5].O.CN1CCOCC1.C(Cl)(=O)OCC.C(O)(C(F)(F)F)=O.[NH2:38][C@H:39]([C:57]([NH2:59])=[O:58])[CH2:40][CH2:41][CH2:42][NH:43][C:44](=[NH:56])[NH:45][S:46]([C:49]1[CH:55]=[CH:54][C:52]([CH3:53])=[CH:51][CH:50]=1)(=[O:48])=[O:47]>CN(C)C=O>[NH:1]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C@@H:2]([C:7]([NH:38][C@H:39]([C:57]([NH2:59])=[O:58])[CH2:40][CH2:41][CH2:42][NH:43][C:44](=[NH:56])[NH:45][S:46]([C:49]1[CH:55]=[CH:54][C:52]([CH3:53])=[CH:51][CH:50]=1)(=[O:48])=[O:47])=[O:9])[CH2:3][CH:4]([CH3:5])[CH3:6]

参加物

7

反応物 5

HCID 6422Trifluoroacetic acidHCID 79724-Methylmorpholine2 回HCID 10928Ethyl chloroformateHCID 2724763D-Leucine, N-[(1,1-dimethylethoxy)carbonyl]-, monohydrateHCID 178427507HCID 178427507、化合物

生成物 1

HCID 178427526HCID 178427526、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
-20 °C

実験手順

2.493 g of Boc-D-Leu-OH.H2O was dissolved in 10 ml of dimethylformamide. The solution was cooled to -20° C. 1.1 ml of N-methylmorpholine and 0.96 ml of ethyl chlorocarbonate were added to the solution. After 5 min, a solution of 4.414 g of CF3COOH.H-Arg(Tos)-NH2 and 1.65 ml of N-methylmorpholine in 20 ml of dimethylformamide was added thereto and the mixture was stirred at about -5° C. for 2 h. After concentration, the residue was dissolved in ethyl acetate and washed with NaHCO3 and water successively. After concentration, ether was added thereto to solidify the product. Thus, 4.96 g of Boc-D-Leu-Arg(Tos)-NH2 was obtained.

後処理

  1. concentrationAfter concentration
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with NaHCO3 and water successively
  4. concentrationAfter concentration, ether
  5. additionwas added

出典と根拠

ORDレコード
ord-6ad2ba2a38aa4476a4a8fdce6e0a6f16
出典データセット
uspto-grants-1987_11
特許番号
US04707468

反応ノート

読み込み中…