Hydrochloric Acid → HCID 178527985, 화합물

HRID 386390

반응식

HRID 386390 반응식
[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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 110801-Naphthyl IsothiocyanateHCID 33557Sodium Azide

생성물 1

HCID 178527985HCID 178527985, 화합물수율 85%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
79 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-c8da1addf57740abb8024f26521d5f0c
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372807B2

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