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Potassium Carbonate → tert-butyl N-[(1Z,2S)-1-amino-3-cyclopropyl-1-hydroxyiminopropan-2-yl]carbamate

HRID 927414
ノート
印刷プレビュー

反応式

HRID 927414 の反応式
C(=O)([O-])[O-].[K+].[K+].Cl.[NH2:8][OH:9].[C:10]([C@@H:12]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:13][CH:14]1[CH2:16][CH2:15]1)#[N:11]>O.C(O)C>[NH2:11]/[C:10](=[N:8]\[OH:9])/[C@@H:12]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:21])([CH3:23])[CH3:22])[CH2:13][CH:14]1[CH2:16][CH2:15]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 71087345(S)-tert-Butyl 1-cyano-2-cyclopropylethylcarbamate

生成物 1

HCID 89262365tert-butyl N-[(1Z,2S)-1-amino-3-cyclopropyl-1-hydroxyiminopropan-2-yl]carbamate収率 94%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 962
Water
溶媒

実験手順

Potassium carbonate (2.18 g, 16 mmol) was dissolved in water (8 mL) and hydroxylamine hydrochloride (1.1 g, 16 mmol) was added. A solution of (S)-tert-butyl 1-cyano-2-cyclopropylethylcarbamate (3.31 g, 16 mmol) in ethanol (24 mL) was added thereto and the resulting reaction mixture was stirred for 72 h. After evaporation of solvents, the residue was dissolved with ethyl acetate (20 mL) and then filtered. The filtrate was concentrated to yield crude product as yellow solid (3.61 g, 94%); MS (EI): m/e 244.2 [M+H]+.

後処理

  1. customthe resulting reaction mixture
  2. customAfter evaporation of solvents
  3. dissolutionthe residue was dissolved with ethyl acetate (20 mL)
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-a18fa72d740f486aa58238a437e81328
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290451B2

反応ノート

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