Toluene → L-aspartyl-L-phenylalanine methyl ester hydrochloride dihydrate

HRID 1583897

反応式

HRID 1583897 の反応式
[CH3:1][O:2][C:3](=[O:27])[C@H:4]([CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[NH:5][C:6](=[O:19])[C@H:7]([CH2:15][C:16](=[O:18])[OH:17])[NH:8]C(=O)CC(C)=O.C1(C)C=CC=CC=1.[ClH:35].N[OH:37]>O.C(O)(=O)C>[OH2:2].[OH2:37].[ClH:35].[CH3:1][O:2][C:3](=[O:27])[C@H:4]([CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[NH:5][C:6](=[O:19])[C@H:7]([CH2:15][C:16](=[O:17])[OH:18])[NH2:8]

参加物

6

反応物 3

HCID 1140TolueneHCID 443297Hydroxyamine hydrochlorideHCID 13334676N-acetoacetyl-L-aspartyl-L-phenylalanine methyl ester

生成物 1

HCID 13020137L-aspartyl-L-phenylalanine methyl ester hydrochloride dihydrate

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

The crude N-acetoacetyl-L-aspartyl-L-phenylalanine methyl ester was dissolved in 100 parts by volume of water and 11.7 parts by volume of acetic acid. Toluene, 200 parts by volume, and hydroxylamine hydrochloride, 6.95 parts by volume, were added and the mixture stirred for 2.5 hours. The aqueous layer was separated and cooled to 0°-5° C. 15 parts by volume concentrated hydrochloric acid were added and the resulting mixture was cooled at 0°-5° C. overnight. The precipitate was collected on a filter and air dried for 3 hours to give 26.4 parts of α-L-aspartyl-L-phenylalanine methyl ester hydrochloride dihydrate.

後処理

  1. customThe aqueous layer was separated
  2. temperaturecooled to 0°-5° C
  3. addition15 parts by volume concentrated hydrochloric acid were added
  4. temperaturethe resulting mixture was cooled at 0°-5° C. overnight
  5. customThe precipitate was collected on
  6. filtrationa filter
  7. customair dried for 3 hours

出典と根拠

ORDレコード
ord-f3e3adb7087f4835af9484840d256308
出典データセット
uspto-grants-1985_11
特許番号
US04555362

関連ノート

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