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Hydroxyamine hydrochloride → HCID 53780880、化合物

HRID 330266
ノート
印刷プレビュー

反応式

HRID 330266 の反応式
Cl.[NH2:2][OH:3].C[O-].[Na+].[Na].[CH:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=[CH:10][C:9]=1[S:18]([CH2:21][C:22]#[N:23])(=[O:20])=[O:19]>CO>[OH:3][N:2]=[C:22]([NH2:23])[CH2:21][S:18]([C:9]1[CH:10]=[CH:11][C:12]2[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:8]=1)(=[O:20])=[O:19]
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 4

HCID 443297Hydroxyamine hydrochlorideHCID 2778444(Naphthalene-2-sulfonyl)acetonitrileHCID 5360545SodiumHCID 10942334Sodium Methoxide

生成物 1

HCID 53780880HCID 53780880、化合物収率 80%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

According to General Procedure A, hydroxylamine hydrochloride (2.26 g, 32.5 mmol), was added in one portion to a solution of NaOMe, freshly prepared from sodium (0.75 g, 32.5 mmol) in methanol. The resulting mixture was stirred 1 hour at room temperature, during which time a precipitate was formed. (2-Naphthalenylsulfonyl)acetonitrile (3.0 g, 13.0 mmol), was added in one portion and the resulting mixture heated to reflux a total of 24 hours. The mixture was cooled to room temperature and then to 0° C. to give a precipitate. The precipitate was collected by filtration, washed with water, and dried in vacuo to give a white crystalline solid (2.75 g, 80%) which was of sufficient purity for use in the subsequent reaction.

後処理

  1. customwas formed
  2. temperaturethe resulting mixture heated
  3. temperatureto reflux a total of 24 hours
  4. temperatureThe mixture was cooled to room temperature
  5. customto 0° C. to give a precipitate
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-04908d49d6934560b16e615cd681b2f0
出典データセット
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04895861

反応ノート

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