Hydrochloric Acid → Melphalan

HRID 1411207노트

반응식

HRID 1411207 반응식
Cl.Cl.C[O:4][C:5](=[O:22])[C@H:6]([CH2:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]([CH2:19][CH2:20][Cl:21])[CH2:16][CH2:17][Cl:18])=[CH:11][CH:10]=1)[NH2:7]>>[Cl:18][CH2:17][CH2:16][N:15]([CH2:19][CH2:20][Cl:21])[C:12]1[CH:11]=[CH:10][C:9]([CH2:8][C@@H:6]([C:5]([OH:22])=[O:4])[NH2:7])=[CH:14][CH:13]=1

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 21144469Melphalan Methyl Ester HCl

생성물 1

HCID 460612Melphalan

반응 조건

온도
0 °C

실험 절차

Concentrated hydrochloric acid (425 ml, 5 volume) was added to the crude 4-[bis(2-chloroethyl)-amino]-L-phenylalanine methyl ester hydrochloride (III) obtained in Example 1 and the reaction mixture was heated at 80° C. to 85° C. After completion of the reaction, as monitored by HPLC, the mixture was treated with activated carbon and filtered through hyflo bed. The filtrate was cooled to 0° C. and the pH of the filtrate was adjusted to pH 6.0 by addition of aqueous ammonia solution (450 ml). The product was filtered, washed with water and the wet 4-[bis(2-chloroethyl)-amino]-L-phenylalanine free base (IV) was used as such for preparation of the hydrochloride salt.

후처리

  1. temperaturethe reaction mixture was heated at 80° C. to 85° C
  2. customAfter completion of the reaction
  3. additionthe mixture was treated with activated carbon
  4. filtrationfiltered through hyflo bed
  5. additionthe pH of the filtrate was adjusted to pH 6.0 by addition of aqueous ammonia solution (450 ml)
  6. filtrationThe product was filtered
  7. washwashed with water
  8. customsuch for preparation of the hydrochloride salt

출처 및 근거

ORD 기록
ord-2a31ad48d6b14cc0811c03628a5b6f67
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921596B2

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