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Sodium Hydroxide → HCID 54030461, 화합물

HRID 1374982
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HRID 1374982 반응식
[C:1]([NH:4][CH:5]([C:16]([OH:18])=[O:17])[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[C:9]([O:14][CH3:15])[CH:8]=1)(=[O:3])[CH3:2].[OH-].[Na+]>O.O.O.O.O.O.[Co](Cl)Cl.O>[C:1]([NH:4][C@@H:5]([C:16]([OH:18])=[O:17])[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[C:9]([O:14][CH3:15])[CH:8]=1)(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium Hydroxide2회HCID 17851043HCID 17851043, 화합물

생성물 1

HCID 54030461HCID 54030461, 화합물수율 37.1%

시약·촉매·용매 2

HCID 517166Dichlorocobalt hexahydrate촉매2회HCID 962Water용매

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온도
37 °C

실험 절차

N-Acetyl-3-methoxy-4-methyl-DL-phenylalanine (7.28 g) was dissolved into a mixture of water (36.5 ml) and 1N sodium hydroxide solution (29 ml). Cobalt(II) chloride hexahydrate (36.5 mg) and acylase (Acylase Amano, 365 mg) were added to the solution and the mixture was stirred at 37° C. for 15.5 hours with controlling the pH of the reaction mixture to 7.5 with 1N sodium hydroxide solution. The insoluble material was removed by filtration and the pH of the filtrate was made to 3 with 6N hydrochloric acid, extracted with ethyl acetate, washed with water, dried over sodium sulfate, and evaporated in vacuo to give crude N-acetyl-3-methoxy-4-methyl-D-phenylalanine (3.17 g). The crude product was again subjected to the acylase reaction (cobalt(II) chloride hexahydrate 15.2 mg, acylase 152 mg, 37° C., pH 7.5, 20 hours) to give pure N-acetyl-3-methoxy-4-methyl-D-phenylalanine (2.70 g) as a viscous oil.

후처리

  1. customThe insoluble material was removed by filtration
  2. extractionextracted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo
  6. customto give crude N-acetyl-3-methoxy-4-methyl-D-phenylalanine (3.17 g)

출처 및 근거

ORD 기록
ord-164a05fad17d42558ce0e3a148c498c9
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07166598B2

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