Formic Acid → Norleucine hydrochloride

HRID 224954ノート

反応式

HRID 224954 の反応式
C[O:2][C:3](=[O:14])[CH:4]([NH:9]C(OC)=O)[CH2:5][CH2:6][CH2:7][CH3:8].[ClH:15].C(O)=O>O>[ClH:15].[NH2:9][CH:4]([C:3]([OH:14])=[O:2])[CH2:5][CH2:6][CH2:7][CH3:8]

参加物

5

反応物 3

HCID 284Formic AcidHCID 313Hydrochloric AcidHCID 536557612-Methoxycarbonylaminohexanoic acid methyl ester

生成物 1

HCID 17985082Norleucine hydrochloride収率 97.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4.07 grams of 2-methoxycarbonylaminohexanoic acid methyl ester were heated in 15 ml of a mixture consisting of equal parts of concentrated hydrochloric acid, 100 weight percent formic acid and water for 24 hours under reflux. The acid mixture was removed in a vacuum, the oily residue treated twice with 20 ml of acetone and freed from acetone again in a vacuum. The now crystalline residue was intensively stirred with 10 ml of acetone, filtered with suction and dried over diphosphorus pentoxide. There were obtained 3.26 grams (97.3%) of D,L-norleucine hydrochloride pure by thin layer chromatography.

後処理

  1. temperatureunder reflux
  2. customThe acid mixture was removed in a vacuum
  3. additionthe oily residue treated twice with 20 ml of acetone
  4. filtrationfiltered with suction
  5. dry with materialdried over diphosphorus pentoxide

出典と根拠

ORDレコード
ord-b4d671eedc4d4d609646148a8645eb0a
出典データセット
uspto-grants-1980_11
特許番号
US04234744

反応ノート

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