Ammonia → HCID 21876582, 화합물

HRID 723786노트

반응식

HRID 723786 반응식
[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

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 962WaterHCID 9964829HCID 9964829, 화합물

생성물 1

HCID 21876582HCID 21876582, 화합물수율 98.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d567f90fb43f409d8a449f3ba5ba9c2f
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07141583B2

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