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Triethylamine → HCID 20406198, 화합물

HRID 2164306
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HRID 2164306 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[C:9]([C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=1)=[O:10].[CH2:18]([S:21][CH2:22][C:23]([NH2:25])=[O:24])[CH2:19][CH3:20].C(OCl)(C)(C)C.C(N(CC)CC)C>C(Cl)Cl>[NH2:1][C:2]1[C:3]([C:9](=[O:10])[C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)=[CH:4][C:5]([CH3:8])=[CH:6][C:7]=1[CH:22]([S:21][CH2:18][CH2:19][CH3:20])[C:23]([NH2:25])=[O:24]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 8471TriethylamineHCID 521297Tert-Butyl hypochloriteHCID 10966280Methanone, (2-amino-5-methylphenyl)(4-fluorophenyl)-HCID 21196834HCID 21196834, 화합물

생성물 1

HCID 20406198HCID 20406198, 화합물수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

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온도
-70 °C

실험 절차

To a mixture of 45.8 g (0.2 mole) of (2-amino-5-methylphenyl)(4-fluorophenyl)methanone and 26.6 g (0.2 mole) of 2-(1-propylthio)acetamide and 700 ml of methylene chloride cooled to -70° C. was added 23 g (0.2 mole) of 95% t-butoxychloride over a 40 minute period. The mixture was kept at -70° C. for 2 additional hours and then 21 g (0.2 mole of triethylamine was added dropwise. The mixture was allowed to warm to room temperature and was washed with water. The organic layer was concentrated and the residue was triturated with isopropyl ether to give 61.7 g (86%) of the titled compound as yellow crystals, m.p. 130.5°-132.5° C.

후처리

  1. customwas kept at -70° C. for 2 additional hours
  2. temperatureto warm to room temperature
  3. washwas washed with water
  4. concentrationThe organic layer was concentrated
  5. customthe residue was triturated with isopropyl ether

출처 및 근거

ORD 기록
ord-a6f3b04eff6a45fc9660fe2e28882def
출처 데이터셋
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04503073

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