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

HRID 263204ノート

反応式

HRID 263204 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 65473Sulbenox

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-9ec13b53c99144ecbcbcf3381ea73987
出典データセット
uspto-grants-1979_05
特許番号
US04156670

反応ノート

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