Hydrochloric Acid → HCID 178527985、化合物

HRID 386390

反応式

HRID 386390 の反応式
[C:1]1([N:11]=[C:12]=[S:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[N-:14]=[N+:15]=[N-:16].[Na+].Cl>C(O)C>[C:1]1([N:11]2[C:12]([SH:13])=[N:16][N:15]=[N:14]2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 110801-Naphthyl IsothiocyanateHCID 33557Sodium Azide

生成物 1

HCID 178527985HCID 178527985、化合物収率 85%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
79 °C

実験手順

To a solution of 1-naphthalenylisothiocyanate (500 mg, 2.7 mmol) in ethanol (150 mL) was added sodium azide (2.8 g, 43 mmol) and the mixture was heated to 79° C. for 2 hours. The reaction mixture was then cooled to room temperature, aqueous HCl solution (12N, 1.5 mL) added and the mixture concentrated. The resulting residue was diluted with ethyl acetate and extracted with aqueous NaOH solution (1N) and the aqueous layer acidified with aqueous HCl solution (12N) until a precipitate formed. The precipitate was collected and used in the next step without further purification (520 mg, 85% yield).

後処理

  1. temperatureThe reaction mixture was then cooled to room temperature
  2. concentrationthe mixture concentrated
  3. additionThe resulting residue was diluted with ethyl acetate
  4. extractionextracted with aqueous NaOH solution (1N)
  5. customformed
  6. customThe precipitate was collected
  7. customused in the next step without further purification (520 mg, 85% yield)

出典と根拠

ORDレコード
ord-c8da1addf57740abb8024f26521d5f0c
出典データセット
uspto-grants-2013_02
特許番号
US08372807B2

関連ノート

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