Dichloromethane → 1H-Imidazole-1-carboxylic acid, 4-[(aminooxy)methyl]-, 1,1-dimethylethyl ester

HRID 330966ノート

反応式

HRID 330966 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[O:12][CH2:13][C:14]1[N:15]=[CH:16][N:17]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH:18]=1.C(Cl)Cl.O.NN>C(O)C>[NH2:3][O:12][CH2:13][C:14]1[N:15]=[CH:16][N:17]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH:18]=1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 24654Hydrazine hydrate (1:1)HCID 86693986HCID 86693986、化合物

生成物 1

HCID 866939871H-Imidazole-1-carboxylic acid, 4-[(aminooxy)methyl]-, 1,1-dimethylethyl ester収率 51%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of tert-butyl 4-{[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]methyl}-1H-imidazole-1-carboxylate 121 (1.72 g, 5.00 mmol) in a solution of DCM (20 mL) and ethanol (4 mL) was added hydrazine hydrate (0.287 mL, 5.00 mmol) at room temperature. The mixture was stirred at room temperature overnight, filtered and concentrated to provide a residue which was washed with ether and methanol to give 122 (0.54 g, 51%) as a white solid.

後処理

  1. filtrationfiltered
  2. concentrationconcentrated
  3. customto provide a residue which
  4. washwas washed with ether and methanol

出典と根拠

ORDレコード
ord-46e2b27df68145f6bc3dffc66820f7e3
出典データセット
uspto-grants-2014_11
特許番号
US08877743B2

反応ノート

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