Phosphorus oxychloride → 11-Chlorodibenzo(b,f)(1,4)thiazepine

HRID 625176

反応式

HRID 625176 の反応式
[CH:1]1[C:6]2[C:7](=O)[NH:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[S:11][C:5]=2[CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:7]1[C:6]2[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=2[S:11][C:10]2[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=2[N:8]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 374829Dibenzothiazepinone

生成物 1

HCID 1058648111-Chlorodibenzo(b,f)(1,4)thiazepine

実験手順

A solution of dibenzo[b,f][1,4]thiazepin-11(10H)-one, prepared as described in the previous step, (14.6 g, 64 mmol) in phosphorus oxychloride (20 mL) was heated to reflux for 2 hours. The mixture was concentrated to provide the crude product which was used directly without further purification. ESI-MS (M+1): 246 calc. for C13H8ClNS 245.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. concentrationThe mixture was concentrated

出典と根拠

ORDレコード
ord-5495f8c0b4b64c369589c5d5e38250a4
出典データセット
uspto-grants-2016_04
特許番号
US09304126B2

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