Hydrazine hydrate (1:1) → tert-Butyl (S)-(1-(aminooxy)propan-2-yl)carbamate

HRID 1053348ノート

反応式

HRID 1053348 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[O:12][CH2:13][C@@H:14]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH3:15].O.NN>C(O)C.C(Cl)Cl>[NH2:3][O:12][CH2:13][C@@H:14]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH3:15]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 86693954tert-Butyl {(1S)-2-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]-1-methylethyl}carbamate

生成物 1

HCID 39238211tert-Butyl (S)-(1-(aminooxy)propan-2-yl)carbamate収率 77.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl {(1S)-2-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]-1-methylethyl}carbamate 58 (1.2 g, 3.74 mmol) in a mixture of ethanol (3 mL) and DCM (20 mL) was added hydrazine hydrate (0.215 mL, 3.74 mmol). The reaction mixture was stirred at room temperature for 6 h. Precipitate was filtered off, the filtrate was evaporated and the residue was subjected to chromatography to give 59 (0.55 g, 77%) as a white solid.

後処理

  1. filtrationPrecipitate was filtered off
  2. customthe filtrate was evaporated

出典と根拠

ORDレコード
ord-413534b9a7b64255a6c7c3ee5f78b0fb
出典データセット
uspto-grants-2016_07
特許番号
US09393239B2

反応ノート

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