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Tetrahydrofuran → 2-(2-Tert-butoxycarbonylaminomethylthiophen-5-yl)carbonyl-4-chloroaniline

HRID 275854
ノート
印刷プレビュー

反応式

HRID 275854 の反応式
O1CCCC1.CN(OC)[C:8](=[O:17])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[NH2:16].Br[C:21]1[S:22][C:23]([CH2:26][NH:27][C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])=[CH:24][CH:25]=1.C([Li])CCC>C(OC(=O)C)C.O.CCCCCC>[C:31]([O:30][C:28]([NH:27][CH2:26][C:23]1[S:22][C:21]([C:8]([C:9]2[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=2[NH2:16])=[O:17])=[CH:25][CH:24]=1)=[O:29])([CH3:34])([CH3:32])[CH3:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8028TetrahydrofuranHCID 2779810tert-Butyl ((5-bromothiophen-2-yl)methyl)carbamateHCID 222266052-amino-5-chloro-N-methoxy-N-methylbenzamideHCID 178418339Butyllithium

生成物 1

HCID 183153332-(2-Tert-butoxycarbonylaminomethylthiophen-5-yl)carbonyl-4-chloroaniline収率 7.3%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8058Hexane溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A tetrahydrofuran (60 ml) solution of N-methyl-N-methyloxy-2-amino-5-chlorobenzamide (4.96 g) and 2-bromo-5-tert-butoxycarbonylaminomethylthiophene (5.45 g) was cooled to −78° C. To the solution was gradually added dropwise a hexane solution of n-butyl lithium (1.6 mol/L) (47 ml). To the mixture were further added water (200 ml) and acetic acid ethyl ester (200 ml). The organic layer was washed with water and dried over anhydrous MgSO4, followed by distilling off the solvent. The residual oily compound was purified by means of a silica gel column chromatography to give 2-(2-tert-butoxycarbonylaminomethylthiophen-5-yl)carbonyl-4-chloroaniline (0.5 g) as a yellow oily product. To a methanol (8 ml) solution of this product (0.15 g) was added sodium borohydride (60 mg). The mixture was stirred for 30 minutes at room temperature, to which was added acetic acid ethyl ester (100 ml). The mixture was washed with water and dried over anhydrous MgSO4. The solvent was then distilled off. To a methanol (5 ml) solution of the residue were added 4-biphenylcarbaldehyde (100 mg) and acetic acid (40 mg). The mixture was stirred for 10 minutes at room temperature, to which was added sodium cyano borohydride (40 mg). The mixture was stirred for 30 minutes at 60° C., to which was added acetic acid ethyl ester (50 ml). The mixture was washed with water and dried over anhydrous MgSO4. The solvent was then distilled off to leave 0.2 g of a residual compound.

後処理

  1. washThe organic layer was washed with water
  2. dry with materialdried over anhydrous MgSO4
  3. distillationby distilling off the solvent
  4. customThe residual oily compound was purified by means of a silica gel column chromatography

出典と根拠

ORDレコード
ord-78487c25e3104edaabeb6a076bdcb343
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06352982B1

反応ノート

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