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Water → HCID 22105454, 화합물

HRID 358039
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HRID 358039 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:12][C:11](=[O:13])[CH2:10][CH2:9]S(=O)(=O)[CH:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[F:22])[C:6]=2[CH:23]=1.C(O)(C)(C)C.O>C(Cl)(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:12][C:11](=[O:13])[CH2:10][CH:9]=[C:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[F:22])[C:6]=2[CH:23]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 6386tert-ButanolHCID 20449977HCID 20449977, 화합물

생성물 1

HCID 22105454HCID 22105454, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

반응 조건

온도
35 °C

실험 절차

67.0 g of 8-chloro-6-(2-fluorophenyl)-1,3,4,6-tetrahydro-2-oxo-2H-5,1-benzothiazocine 5,5-dioxide are suspended in a mixture of 670 ml of carbon tetrachloride, 670 ml of t-butanol and 31.5 ml of water. The suspension is pre-warmed to 35° C. There are then rapidly added thereto while cooling four 51.5 g portions of potassium t-butylate (the temperature amounts to 45°-50°). The mixture is stirred for a further 35 minutes, the temperature dropping to about 35°. The mixture is poured on to ice, whereupon it is extracted with methylene chloride. The organic phase is evaporated and the residue is triturated with ether. The crystalline product is filtered off. There is obtained 7-chloro-5-(2-fluorophenyl)-1,3-dihydro-2H-1-benzazepin-2-one of melting point 214°-215°.

후처리

  1. additionThere are then rapidly added
  2. customamounts to 45°-50°
  3. customdropping to about 35°
  4. additionThe mixture is poured on to ice, whereupon it
  5. extractionis extracted with methylene chloride
  6. customThe organic phase is evaporated
  7. customthe residue is triturated with ether
  8. filtrationThe crystalline product is filtered off

출처 및 근거

ORD 기록
ord-ef4cddb03ffb4a1787733283cb4904f8
출처 데이터셋
uspto-grants-1984_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04464300

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