Hydrochloric Acid → 8-Fluoro-10-hydroxy-10,11-dihydrodibenzo[b,f]thiepin-3-carboxylic Acid

HRID 485470ノート

反応式

HRID 485470 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=[C:13]([C:16]([OH:18])=[O:17])[CH:14]=[CH:15][C:9]=3[CH2:8][C:7](=[O:19])[C:6]=2[CH:20]=1.C(=O)(O)[O-].[Na+].[BH4-].[Na+].Cl>O>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=[C:13]([C:16]([OH:18])=[O:17])[CH:14]=[CH:15][C:9]=3[CH2:8][CH:7]([OH:19])[C:6]=2[CH:20]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 1303510610-Oxo-8-fluoro-dibenzo[b,f]thiepin-3-carboxylic acid

生成物 1

HCID 134904028-Fluoro-10-hydroxy-10,11-dihydrodibenzo[b,f]thiepin-3-carboxylic Acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

Suspend 15.5 gm of the crude 10-keto compound of Step B in 750 ml of water and add 10 gm of sodium bicarbonate. Stir the mixture and warm to 50° C. for 15-20 minutes. Stop heating and slowly add 5 gm of sodium borohydride. Acidify the mixture with 10% aqueous hydrochloric acid, separate the solids by filtration, wash with water and air-dry. The residue may be used as such in the next step. (m.p. 204°-210° C., subsequent gassing)

後処理

  1. temperatureStop heating
  2. customseparate the solids
  3. filtrationby filtration
  4. washwash with water
  5. customair-dry

出典と根拠

ORDレコード
ord-4938c9c22f6b40ccb63fe12a658b6011
出典データセット
uspto-grants-1985_08
特許番号
US04536507

反応ノート

読み込み中…