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Water → HCID 7408430、化合物

HRID 2209861
ノート
印刷プレビュー

反応式

HRID 2209861 の反応式
[NH:1](C(OCC1C=CC=CC=1)=O)[C@H:2]([C:28]([OH:30])=[O:29])[CH2:3][CH2:4][C:5](=[O:27])[NH:6][C:7]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:8]1[CH:14]=[CH:13][C:11]([CH3:12])=[CH:10][CH:9]=1.O>CO.Cl.[Pd]>[NH2:1][C@H:2]([C:28]([OH:30])=[O:29])[CH2:3][CH2:4][C:5](=[O:27])[NH:6][C:7]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:8]1[CH:14]=[CH:13][C:11]([CH3:12])=[CH:10][CH:9]=1
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 2

HCID 962WaterHCID 90470049(S)-2-(((Benzyloxy)carbonyl)amino)-5-((diphenyl(p-tolyl)methyl)amino)-5-oxopentanoic acid

生成物 1

HCID 7408430HCID 7408430、化合物収率 85%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 313Hydrochloric Acid溶媒HCID 887
Methanol
溶媒

実験手順

A suspension of 107.3 g Z-Gln(Mtt)OH (200 mM) in 800 ml methanol and 200 ml IN hydrochloric acid is hydrogenated at room temperature and normal pressure in the presence of 0.4 g palladium on carbon (10%) catalyst. On completion of the hydrogen uptake the catalyst is filtered off, washed with methanol and the filtrate, after addition of 27.9 ml triethylamine (200 mM) and 200 ml water, concentrated to a volume of about 600 ml. The formed crystalline precipitate is filtered off and washed with water until the washings are chloride-free. The obtained H-Gln(Mtt)OH contains 0.5-1 mole water and decomposes slowly above 231° C. Yield 85%.

後処理

  1. customis hydrogenated at room temperature
  2. filtrationOn completion of the hydrogen uptake the catalyst is filtered off
  3. washwashed with methanol
  4. additionthe filtrate, after addition of 27.9 ml triethylamine (200 mM) and 200 ml water
  5. concentrationconcentrated to a volume of about 600 ml
  6. filtrationThe formed crystalline precipitate is filtered off
  7. washwashed with water until the washings
  8. customdecomposes slowly above 231° C

出典と根拠

ORDレコード
ord-66c4307aa86b453bb77f61fbf565f916
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05455363

反応ノート

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