Hydrochloric Acid → N-(tert-Butoxycarbonyl)-3,4-dibenzyloxyphenylalanine

HRID 1587181

반응식

HRID 1587181 반응식
C([O:8][C:9](=[O:42])[C@H:10]([CH2:19][C:20]1[CH:25]=[CH:24][C:23]([O:26][CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)=[C:22]([O:34][CH2:35][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:21]=1)[NH:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])C1C=CC=CC=1.[OH-].[Na+].O.Cl>CO>[C:15]([O:14][C:12]([NH:11][C@H:10]([C:9]([OH:42])=[O:8])[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([O:26][CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)=[C:22]([O:34][CH2:35][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:21]=1)=[O:13])([CH3:18])([CH3:16])[CH3:17]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 22976099N-(tert-Butoxycarbonyl)-3,4-dibenzyloxyphenylalanine benzyl ester

생성물 1

HCID 12968276N-(tert-Butoxycarbonyl)-3,4-dibenzyloxyphenylalanine수율 99.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

30.0 g of the crystals obtained in Example 4 was dissolved in 600 ml of methanol, and after the addition of 65 ml of 10% sodium hydroxide, the mixture was stirred at a room temperature for 20 hours, and 1000 ml of water was added. The reaction mixture was adjusted to pH 4 with concentrated hydrochloric acid, and extracted twice with 800 ml of chloroform. The extract was dried over magnesium sulfate and concentrated under a reduced pressure to crystallize the title compound, which was then filtered and washed with hexane to obtain 25.2 g of colorless crystals.

후처리

  1. extractionextracted twice with 800 ml of chloroform
  2. dry with materialThe extract was dried over magnesium sulfate
  3. concentrationconcentrated under a reduced pressure
  4. customto crystallize the title compound, which
  5. filtrationwas then filtered
  6. washwashed with hexane

출처 및 근거

ORD 기록
ord-3994e06923094b70b6ffa721a47b8dfa
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05216150

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