Dimethyl Sulfoxide → HCID 86613082、化合物

HRID 1869142ノート

反応式

HRID 1869142 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 86613082HCID 86613082、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

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)

後処理

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

出典と根拠

ORDレコード
ord-442f9b5429fc411da1fb88fd74b5be14
出典データセット
uspto-grants-2009_12
特許番号
US07638514B2

反応ノート

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