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Hydrazine hydrate (1:1) → 2-{[4-(3-Aminopropyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid tert-butyl ester

HRID 914291
ノート
印刷プレビュー

反応式

HRID 914291 の反応式
[C:1]([O:5][C:6](=[O:30])[C:7]([CH3:29])([S:9][C:10]1[S:11][CH:12]=[C:13]([CH2:15][CH2:16][CH2:17][N:18]2C(=O)C3=CC=CC=C3C2=O)[N:14]=1)[CH3:8])([CH3:4])([CH3:3])[CH3:2].O.NN>C(O)C>[C:1]([O:5][C:6](=[O:30])[C:7]([S:9][C:10]1[S:11][CH:12]=[C:13]([CH2:15][CH2:16][CH2:17][NH2:18])[N:14]=1)([CH3:29])[CH3:8])([CH3:3])([CH3:2])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 597588132-Methyl-2-{[4-(3-phthalimidopropyl)-1,3-thiazol-2-yl]thio}propionic acid tert-butyl ester

生成物 1

HCID 597590072-{[4-(3-Aminopropyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid tert-butyl ester収率 91.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Methyl-2-{[4-(3-phthalimidopropyl)-1,3-thiazol-2-yl]thio}propionic acid tert-butyl ester (31.1 g) obtained in Example 32 was dissolved in ethanol (400 mL), hydrazine monohydrate (10 mL) was added, and the mixture was refluxed for 2 hr. The precipitated solid was removed by filtration, and the filtrate was concentrated under reduced pressure. Water and dichloromethane were added to the residue, and the organic layer was washed with water, and dried over magnesium sulfate. The solvent was concentrated under reduced pressure to give the title compound (20.1 g). The obtained compound was used in the next reaction without purification.

後処理

  1. temperaturethe mixture was refluxed for 2 hr
  2. customThe precipitated solid was removed by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionWater and dichloromethane were added to the residue
  5. washthe organic layer was washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationThe solvent was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-6bafd0e3d75e438c9c43fae065e9bc71
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08026370B2

反応ノート

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