Hydrochloric Acid → HCID 66918867、化合物

HRID 1006550ノート

反応式

HRID 1006550 の反応式
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:6]=1[N:15]([S:19]([CH2:22][CH:23](O)[CH2:24][CH2:25][CH2:26][CH3:27])(=[O:21])=[O:20])[CH:16]([CH3:18])[CH3:17].N12CCCCC1CNCC=C2.Cl>C(Cl)Cl.C(N(CC)CC)C.S(Cl)(C)(=O)=O>[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:6]=1[N:15]([S:19]([CH:22]=[CH:23][CH2:24][CH2:25][CH2:26][CH3:27])(=[O:20])=[O:21])[CH:16]([CH3:18])[CH3:17]

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 22671994HCID 22671994、化合物HCID 226720701,5-Diazabicyclo[5.4.0]undecene

生成物 1

HCID 66918867HCID 66918867、化合物収率 91.3%

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒HCID 31297Methanesulfonyl chloride溶媒

実験手順

To a solution of 2-(N-isopropyl-2-hydroxyhexylsulfonylamino)-5-trifluoromethylphenyl methoxymethyl ether (160 mg; prepared in Reference Example 31) in methylene chloride (2.0 ml), triethylamine (104 μl) and mesylchloride (35 μl) were added in a stream of argon at 0° C. The mixture was stirred for 10 minutes. To the mixture, 1,5-diazabicyclo[5,4,0]undecene (134 μl) was added. The mixture was stirred for 2 hours at room temperature. To the reaction mixture, diluted HCl was added. The mixture was extracted with ethyl acetate, washed, dried over and concentrated with the reduced pressure. The residue was purified on silica gel column chromatography (hexane:AcOEt=8:1) to give the title compound (140 mg) having the following physical data.

後処理

  1. stirringThe mixture was stirred for 2 hours at room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. washwashed
  4. customdried over and
  5. concentrationconcentrated with the reduced pressure
  6. customThe residue was purified on silica gel column chromatography (hexane:AcOEt=8:1)

出典と根拠

ORDレコード
ord-9393d9b48c824cb8bfebf347ea3da549
出典データセット
uspto-grants-2004_09
特許番号
US06790866B2

反応ノート

読み込み中…