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Sodium Hydroxide → 2-ethylsulfanyl-N-[(3-fluorophenyl)-methyl]-6-methyl-4-morpholin-4-yl-benzamide

HRID 515143
ノート
印刷プレビュー

反応式

HRID 515143 の反応式
[CH2:1]([S:3][C:4]1[CH:12]=[C:11]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)[CH:10]=[C:9]([CH3:19])[C:5]=1[C:6]([NH2:8])=[O:7])[CH3:2].[OH-].[Na+].[F:22][C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[CH2:26]Br>C1C=CC=CC=1.O1CCCC1.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C1C=CC=CC=1.O>[CH2:1]([S:3][C:4]1[CH:12]=[C:11]([N:13]2[CH2:14][CH2:15][O:16][CH2:17][CH2:18]2)[CH:10]=[C:9]([CH3:19])[C:5]=1[C:6]([NH:8][CH2:26][C:25]1[CH:28]=[CH:29][CH:30]=[C:23]([F:22])[CH:24]=1)=[O:7])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 14798Sodium HydroxideHCID 680073-Fluorobenzyl bromideHCID 866997242-Ethylsulfanyl-6-methyl-4-morpholin-4-yl-benzamide

生成物 1

HCID 721877892-ethylsulfanyl-N-[(3-fluorophenyl)-methyl]-6-methyl-4-morpholin-4-yl-benzamide収率 16%

試薬・触媒・溶媒 4

HCID 94433Tetrabutylammonium hydrogen sulfate触媒
HCID 241
Benzene
溶媒
HCID 962Water溶媒
HCID 22633675Benzene tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

To a solution of 2-ethylsulfanyl-6-methyl-4-morpholin-4-yl-benzamide (0.26 g, 0.92 mmol) in benzene-tetrahydrofuran (1:1) (20 ml) are added tetrabutylammonium hydrogensulfate (0.031 g, 0.091 mmol) and 50% sodium hydroxide solution (8 ml) at RT. The reaction mixture is heated to 80° C. and 3-fluorobenzyl bromide (0.14 ml of a 2M solution in benzene, 0.28 mmol) is added. The reaction mixture is stirred at 80° C. for 15 min. After completion of the reaction (monitored by TLC), the reaction mixture is diluted with water (15 ml) and extracted with ethyl acetate (15×3 ml). The organic layer is washed with water (20 ml), brine (15 ml), dried over anhydrous sodium sulfate and evaporated to get the crude product, which is purified by column chromatography (silica gel, 25% ethyl acetate/hexane) to yield 2-ethylsulfanyl-N-[(3-fluorophenyl)-methyl]-6-methyl-4-morpholin-4-yl-benzamide (example 1) (0.06 g, 0.15 mmol, 16%). [M+H]+ 389.1.

後処理

  1. customAfter completion of the reaction (monitored by TLC)
  2. extractionextracted with ethyl acetate (15×3 ml)
  3. washThe organic layer is washed with water (20 ml), brine (15 ml)
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated
  6. customto get the crude product, which
  7. customis purified by column chromatography (silica gel, 25% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-feb3e339a00a4bd58b1d2ba57e451550
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09108936B2

反応ノート

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