4,5,6,7-Tetrahydro-7-oxobenzo[b]thiophen-4-amine hydrochloride → Sulbenox

HRID 263204노트

반응식

HRID 263204 반응식
Cl.[O:2]=[C:3]1[C:8]2[S:9][CH:10]=[CH:11][C:7]=2[CH:6]([NH2:12])[CH2:5][CH2:4]1.[O:13]([C:15]#[N:16])[K]>O>[O:2]=[C:3]1[C:8]2[S:9][CH:10]=[CH:11][C:7]=2[CH:6]([NH:12][C:15]([NH2:16])=[O:13])[CH2:5][CH2:4]1

참가 물질

4

반응물 2

HCID 233477954,5,6,7-Tetrahydro-7-oxobenzo[b]thiophen-4-amine hydrochlorideHCID 178418250HCID 178418250, 화합물

생성물 1

HCID 65473Sulbenox

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

The aqueous solution (280 ml.) of (+)-4,5,6,7-tetrahydro-7-oxobenzo[b]thiophen-4-amine hydrochloride from Example 53 is stirred while 40 grams of KOCN in 95 ml. of water is added dropwise. The mixture is warmed to 70° C. for 1.5 hour and cooled to 10° C. The light brown solid is collected and washed well with 700 ml. of water. The product is then stirred with 110 ml. of cold methanol, collected, and washed with 50 ml. of cold methanol to afford 48 grams of the title compound, m.p. 247°-249.5° C. (dec.), [α]D24 =-97.16° (c, 0.14 in methanol).

후처리

  1. temperaturecooled to 10° C
  2. customThe light brown solid is collected
  3. washwashed well with 700 ml
  4. customof cold methanol, collected
  5. washwashed with 50 ml

출처 및 근거

ORD 기록
ord-9ec13b53c99144ecbcbcf3381ea73987
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04156670

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