Hydrazine hydrate (1:1) → (S)-2-Amino-5,5-dimethoxypentanoic acid, methyl ester

HRID 52802노트

반응식

HRID 52802 반응식
C1(=O)[N:5]([C@@H:6]([CH2:11][CH2:12][CH:13]([O:16][CH3:17])[O:14][CH3:15])[C:7]([O:9][CH3:10])=[O:8])C(=O)C2=CC=CC=C12.O.NN>CO>[NH2:5][C@@H:6]([CH2:11][CH2:12][CH:13]([O:16][CH3:17])[O:14][CH3:15])[C:7]([O:9][CH3:10])=[O:8]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 10914214(S)-2-Phthalimido-5,5-dimethoxypentanoic acid, methyl ester

생성물 1

HCID 642239(S)-2-Amino-5,5-dimethoxypentanoic acid, methyl ester

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(S)-2-Phthalimido-5,5-dimethoxypentanoic acid, methyl ester [prepared as described in Example 4(f), 3.35 g., 10.43 mmol.) in methanol (70 ml.) was treated with hydrazine monohydrate (531 μl., 10.95 mmol., 1.05 eq.) and the solution was stirred at room temperature for 6 days. The mixture was filtered and the solid was washed with methanol. The filtrate was concentrated, triturated with methylene chloride, filtered again, concentrated, and dried in vacuo to yield 1.89 g. of title product as a cloudy oil. TLC (10% methanol in methylene chloride) Rf =0.39.

후처리

  1. filtrationThe mixture was filtered
  2. washthe solid was washed with methanol
  3. concentrationThe filtrate was concentrated
  4. customtriturated with methylene chloride
  5. filtrationfiltered again
  6. concentrationconcentrated
  7. customdried in vacuo
  8. customto yield 1.89 g

출처 및 근거

ORD 기록
ord-14c6e5346757410bb7f289547b120f39
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616775

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