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

HRID 52802ノート

反応式

HRID 52802 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-14c6e5346757410bb7f289547b120f39
出典データセット
uspto-grants-1997_04
特許番号
US05616775

反応ノート

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