Water → HCID 59634043、化合物

HRID 1615054ノート

反応式

HRID 1615054 の反応式
[CH:1]1([C:4]2[CH:33]=[CH:32][C:7]([CH2:8][O:9][C:10]3[CH:15]=[CH:14][C:13]([CH:16]4[CH2:19][N:18]([C:20]([C:22]5[CH:27]=[C:26]([CH2:28][OH:29])[CH:25]=[CH:24][N:23]=5)=[O:21])[CH2:17]4)=[CH:12][C:11]=3[O:30][CH3:31])=[CH:6][CH:5]=2)[CH2:3][CH2:2]1.C(N(CC)CC)C.[CH3:41][S:42](Cl)(=[O:44])=[O:43].O>C(Cl)(Cl)Cl>[CH3:41][S:42]([O:29][CH2:28][C:26]1[CH:25]=[CH:24][N:23]=[C:22]([C:20]([N:18]2[CH2:17][CH:16]([C:13]3[CH:14]=[CH:15][C:10]([O:9][CH2:8][C:7]4[CH:32]=[CH:33][C:4]([CH:1]5[CH2:3][CH2:2]5)=[CH:5][CH:6]=4)=[C:11]([O:30][CH3:31])[CH:12]=3)[CH2:19]2)=[O:21])[CH:27]=1)(=[O:44])=[O:43]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 59633911HCID 59633911、化合物2 回

生成物 1

HCID 59634043HCID 59634043、化合物収率 99%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of {3-[4-(4-cyclopropylbenzyloxy)-3-methoxyphenyl]azetidin-1-yl}-(4-hydroxymethylpyridin-2-yl)-methanone (4.0 g) prepared in (6) in chloroform (80 mL) were added triethylamine (3.0 mL) and methanesulfonyl chloride (1.5 mL) at 0° C. The reaction mixture was stirred at RT for 30 min. Water was added to the reaction mixture and the mixture was extracted with chloroform. The organic layer was dried over MgSO4. The solvent was removed under reduced pressure. Hexane was added to the residue. The precipitated solid was collected on a filter and dried to give the title compound (4.6 g, 99%).

後処理

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialThe organic layer was dried over MgSO4
  3. customThe solvent was removed under reduced pressure
  4. additionHexane was added to the residue
  5. customThe precipitated solid was collected on
  6. filtrationa filter
  7. customdried

出典と根拠

ORDレコード
ord-186027dec39341bea25df95f6a823632
出典データセット
uspto-grants-2014_07
特許番号
US08765739B2

反応ノート

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