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

HRID 1633385

반응식

HRID 1633385 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

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 6.95 parts of hydroxylamine hydrochloride 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.

후처리

  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

출처 및 근거

ORD 기록
ord-b016a516852d4fdea7a33bbcaa231f3a
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04480112

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