Formic Acid → tert-Butyl {(phenylsulphonyl)[3-(trifluoromethyl)phenyl]methyl}carbamate

HRID 220630

反応式

HRID 220630 の反応式
[C:1](=[O:8])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])[NH2:2].[C:9]1([S:15]([O-:17])=[O:16])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[Na+].[F:19][C:20]([F:30])([F:29])[C:21]1[CH:22]=[C:23]([CH:27]=O)[CH:24]=[CH:25][CH:26]=1.C(O)=O>CO.O>[C:9]1([S:15]([CH:27]([NH:2][C:1](=[O:8])[O:3][C:4]([CH3:7])([CH3:6])[CH3:5])[C:23]2[CH:24]=[CH:25][CH:26]=[C:21]([C:20]([F:19])([F:29])[F:30])[CH:22]=2)(=[O:17])=[O:16])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

6

反応物 4

HCID 284Formic AcidHCID 679903-(Trifluoromethyl)benzaldehydeHCID 77922tert-Butyl carbamateHCID 2723840Benzenesulfinic acid, sodium salt

生成物 1

HCID 59536907tert-Butyl {(phenylsulphonyl)[3-(trifluoromethyl)phenyl]methyl}carbamate

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

A quantity of 4.49 g (38.29 mmol) of tert-butyl carbamate and 12.57 g (76.57 mmol) of sodium benzenesulphinate were introduced in 110 ml of methanol/water 1:2 and admixed in succession with 10 g (57.43 mmol) of 3-(trifluoromethyl)benzenecarbaldehyde and 2.87 ml (76.09 mmol) of formic acid. The mixture was stirred at RT for 30 h. The precipitated product was isolated by filtration, washed in succession with water and diethyl ether and sucked dry. Further drying in an HV gave 11.2 g (47% of theory) of the title compound.

後処理

  1. customThe precipitated product was isolated by filtration
  2. washwashed in succession with water and diethyl ether
  3. customsucked dry
  4. customFurther drying in an HV

出典と根拠

ORDレコード
ord-dd01c49f80e34d9485cb26a159e4f399
出典データセット
uspto-grants-2012_06
特許番号
US08202895B2

関連ノート

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