Methanethiol → phenyl 3-methylthio-N-phenylacrylimidate

HRID 1918445ノート

反応式

HRID 1918445 の反応式
O([CH:8]=[CH:9][C:10](=[N:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)C1C=CC=CC=1.C1COCC1.[Na].[CH3:31][SH:32]>C(OCC)(=O)C>[CH3:31][S:32][CH:8]=[CH:9][C:10](=[N:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

6

反応物 4

HCID 878MethanethiolHCID 8028TetrahydrofuranHCID 5360545SodiumHCID 69127142Phenyl 3-phenoxy-N-phenylacrylimidate

生成物 1

HCID 69126846phenyl 3-methylthio-N-phenylacrylimidate収率 78.1%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Phenyl 3-phenoxy-N-phenylacrylimidate (0.30 g) was dissolved to THF (5 ml), sodium salt of methyl mercaptan (0.075 g) was added thereto and stirred for four hours at room temperature. Ethyl acetate (50 ml) was added to the reaction solution, and it was successively washed with water and aqueous saturated of sodium chloride solution, dried over magnesium sulfate (anhydrous), concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (hexane:ethyl acetate=10:1) to obtain phenyl 3-methylthio-N-phenylacrylimidate (0.20 g) as yellow oil.

後処理

  1. additionwas added
  2. washwas successively washed with water and aqueous saturated of sodium chloride solution
  3. dry with materialdried over magnesium sulfate (anhydrous)
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-c7badc4004d04c9ea4ad6879e96bcc4a
出典データセット
uspto-grants-2013_12
特許番号
US08618329B2

反応ノート

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