Carbon Dioxide → H-His-Lys(Boc)-OMe

HRID 1982307ノート

反応式

HRID 1982307 の反応式
[NH:1](C(OCC1C=CC=CC=1)=O)[C@H:2]([C:9]([NH:11][C@H:12]([C:25]([O:27][CH3:28])=[O:26])[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[O:10])[CH2:3][C:4]1[N:8]=[CH:7][NH:6][CH:5]=1.Cl.C(=O)=O>CO>[NH2:1][C@H:2]([C:9]([NH:11][C@H:12]([C:25]([O:27][CH3:28])=[O:26])[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[O:10])[CH2:3][C:4]1[N:8]=[CH:7][NH:6][CH:5]=1

参加物

5

実験手順

1.6 g of Z-His-Lys(Boc)-OMe [S. Guttman et al., Helv. Chim. Acta 52, 1789 (1969)] are dissolved in 33 ml of MeOH, 3 ml of 1N HCl and 160 mg of Pd-on-carbon (10% pd) are added thereto, and hydrogenation is carried out with CO2 -absorption until saturation. After filtering off the catalyst, the whole is concentrated, the oily residue is dissolved in 20 ml of DMF and again concentrated to approximately 10 ml, yielding H-His-Lys(Boc)-OMe in the form of a solution which is immediately further processed in stage 2.2.

後処理

  1. filtrationAfter filtering off the catalyst
  2. concentrationthe whole is concentrated
  3. dissolutionthe oily residue is dissolved in 20 ml of DMF
  4. concentrationagain concentrated to approximately 10 ml

出典と根拠

ORDレコード
ord-041d176aa1c94211a19bf4f19e787129
出典データセット
uspto-grants-1986_06
特許番号
US04595677

反応ノート

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