Ammonia → HCID 21876582、化合物

HRID 723786ノート

反応式

HRID 723786 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2(O)[CH2:14][CH2:13][S:12][CH2:11][CH2:10]2)=[C:4]([F:16])[CH:3]=1.Cl.O.N>C(O)(=O)C>[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH2:14][CH2:13][S:12][CH2:11][CH:10]=2)=[C:4]([F:16])[CH:3]=1

参加物

6

反応物 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 962WaterHCID 9964829HCID 9964829、化合物

生成物 1

HCID 21876582HCID 21876582、化合物収率 98.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

4-(4-Amino-2,6-difluoro-phenyl)-tetrahydro-thiopyran-4-o1 (16.7 g, 68 mM) was suspended in a mixture of concentrated hydrochloric acid (200 ml), water (50 ml) and acetic acid (200 ml), BHT (50 mg) added, and the whole stirred under nitrogen at 800 for 18 hours. After cooling, the mixture was made basic by cautious addition of concentrated ammonia, and ice-water. The mixture was then extracted with diethyl ether (2×300 ml), the extracts washed with water (100 ml), brine (200 ml) and dried (magnesium sulfate). Evaporation gave the desired product as a cream solid (15.2 g).

後処理

  1. additionadded
  2. temperatureAfter cooling
  3. extractionThe mixture was then extracted with diethyl ether (2×300 ml)
  4. washthe extracts washed with water (100 ml), brine (200 ml)
  5. dry with materialdried (magnesium sulfate)
  6. customEvaporation

出典と根拠

ORDレコード
ord-d567f90fb43f409d8a449f3ba5ba9c2f
出典データセット
uspto-grants-2006_11
特許番号
US07141583B2

反応ノート

読み込み中…