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Hydrazine hydrate (1:1) → (2r)-2-Amino-ethanesulfonic acid (5-chloro-2-{2-[4-(4-fluoro-benzyl)-2-methyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-amide

HRID 480191
ノート
印刷プレビュー

反応式

HRID 480191 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:25][CH2:26][C:27]([N:29]2[CH2:34][CH2:33][N:32]([CH2:35][C:36]3[CH:41]=[CH:40][C:39]([F:42])=[CH:38][CH:37]=3)[CH2:31][CH:30]2[CH3:43])=[O:28])=[C:6]([NH:8][S:9]([CH2:12][CH2:13][N:14]2C(=O)C3C(=CC=CC=3)C2=O)(=[O:11])=[O:10])[CH:7]=1.O.NN>CCO.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:25][CH2:26][C:27]([N:29]2[CH2:34][CH2:33][N:32]([CH2:35][C:36]3[CH:37]=[CH:38][C:39]([F:42])=[CH:40][CH:41]=3)[CH2:31][C@H:30]2[CH3:43])=[O:28])=[C:6]([NH:8][S:9]([CH2:12][CH2:13][NH2:14])(=[O:11])=[O:10])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 699590132-(1,3-Dioxo-1,3-dihydro-isoindol-2-yl)-ethanesulfonic acid (5-chloro-2-{2-[4-(4-fluoro-benzyl)-2-methyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-amide

生成物 1

HCID 12112110(2r)-2-Amino-ethanesulfonic acid (5-chloro-2-{2-[4-(4-fluoro-benzyl)-2-methyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-amide収率 58.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 962
Water
溶媒

実験手順

To a solution of 2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-ethanesulfonic acid (5-chloro-2-{2-[4-(4-fluoro-benzyl)-2-methyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-amide (0.030 g, 0.048 mmol) in EtOH (1 mL) at ambient temperature was added hydrazine hydrate (0.025 mL). The reaction was stirred overnight at ambient temperature then diluted with water and extracted with methylene chloride (2×). The combined organics were washed with saturated aqueous brine and dried over sodium sulfate, filtered and concentrated in vacuo. Purification via radial chromatography (2 mm plate) gave the title compound (0.014 g).

後処理

  1. extractionextracted with methylene chloride (2×)
  2. washThe combined organics were washed with saturated aqueous brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customPurification via radial chromatography (2 mm plate)

出典と根拠

ORDレコード
ord-f715768bd85649cbba57cb407438bbca
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06649611B2

反応ノート

読み込み中…

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