Dimethyl Sulfoxide → HCID 86613082, 화합물

HRID 1869142노트

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HRID 1869142 반응식
CS(C)=O.C(Cl)(=O)C(Cl)=O.[Cl:11][C:12]1[CH:33]=[C:32]([O:34][CH2:35][CH:36]=[C:37]([Cl:39])[Cl:38])[CH:31]=[C:30]([Cl:40])[C:13]=1[O:14][CH2:15][CH:16]([OH:29])[CH2:17][O:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]([F:28])([F:27])[F:26])=[CH:21][CH:20]=1.C(N(CC)CC)C>ClCCl.O>[Cl:11][C:12]1[CH:33]=[C:32]([O:34][CH2:35][CH:36]=[C:37]([Cl:38])[Cl:39])[CH:31]=[C:30]([Cl:40])[C:13]=1[O:14][CH2:15][C:16](=[O:29])[CH2:17][O:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]([F:28])([F:27])[F:26])=[CH:21][CH:20]=1

참가 물질

7

반응물 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 866130811-[2,6-Dichloro-4-(3,3-dichloro-allyloxy)-phenoxy]-3-(4-trifluoromethyl-phenoxy)-propan-2-ol

생성물 1

HCID 86613082HCID 86613082, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

1.15 ml of dimethyl sulfoxide are added at −60° C. in the course of 5 minutes to 0.63 ml of oxalyl chloride in 50 ml of dichloromethane. After 40 minutes, a solution of 3.4 g of 1-[2,6-dichloro-4-(3,3-dichloro-allyloxy)-phenoxy]-3-(4-trifluoromethyl-phenoxy)-propan-2-ol in 30 ml of dichloromethane is added dropwise in the course of 10 minutes. After 40 minutes, 4.5 ml of triethylamine are added and the reaction mixture is slowly heated to room temperature. The reaction mixture is then poured into water and extracted with dichloromethane. After concentration of the organic phase and crystallisation from diethyl ether/hexane, 1-[2,6-dichloro-4-(3,3-dichloro-allyloxy)-phenoxy]-3-(4-trifluoromethyl-phenoxy)-propan-2-one is obtained. 1H-NMR (CDCl3) 300 MHz: 4.61 (d, 2H), 4.74 (s, 2H), 5.21 (s, 2H), 6.12 (t, 1H), 6.90 (s, 2H), 7.11 (d, 2H), 7.59 (d, 2H)

후처리

  1. waitAfter 40 minutes
  2. extractionextracted with dichloromethane
  3. customAfter concentration of the organic phase and crystallisation from diethyl ether/hexane

출처 및 근거

ORD 기록
ord-442f9b5429fc411da1fb88fd74b5be14
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638514B2

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