tert-Butoxy bis(dimethylamino)methane → 7-[(Dimethylamino)methylene]-4,5,6,7-tetrahydro-4-4-nitrobenzyl-8H-thieno[3,2-b]azepin-8-one

HRID 863024ノート

反応式

HRID 863024 の反応式
[N+:1]([C:4]1[CH:22]=[CH:21][C:7]([C:8]([N:10]2[CH2:16][CH2:15][CH2:14][C:13](=[O:17])[C:12]3[S:18][CH:19]=[CH:20][C:11]2=3)=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].C(O[CH:28](N(C)C)[N:29]([CH3:31])[CH3:30])(C)(C)C>>[CH3:28][N:29]([CH:31]=[C:14]1[CH2:15][CH2:16][N:10]([CH2:8][C:7]2[CH:21]=[CH:22][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=2)[C:11]2[CH:20]=[CH:19][S:18][C:12]=2[C:13]1=[O:17])[CH3:30]

参加物

3

反応物 2

HCID 79885tert-Butoxy bis(dimethylamino)methaneHCID 196990654,5,6,7-tetrahydro-4-(4-nitrobenzoyl)-8H-thieno[3,2-b]azepin-8-one

生成物 1

HCID 676622387-[(Dimethylamino)methylene]-4,5,6,7-tetrahydro-4-4-nitrobenzyl-8H-thieno[3,2-b]azepin-8-one

実験手順

A mixture of 3.2 g of 4,5,6,7-tetrahydro-4-(4-nitrobenzoyl)-8H-thieno[3,2-b]azepin-8-one and 32 ml of tert-butoxybis(dimethylamino)methane is heated on a steam bath for 3.5 hours. The reaction mixture is allowed to stand for 48 hours. The reaction mixture is evaporated in vacuo and the concentrate is dissolved in 150 ml of methylene chloride and filtered through hydrous magnesium silicate two times. The volatiles are evaporated in vacuo to a residue which is dissolved in 25 ml of ethyl acetate and filtered. The filtrate is cooled to give 3.2 g of the desired product as a light orange solid, m.p. 214°-216° C.

後処理

  1. temperatureis heated on a steam bath for 3.5 hours
  2. customThe reaction mixture is evaporated in vacuo
  3. dissolutionthe concentrate is dissolved in 150 ml of methylene chloride
  4. filtrationfiltered through hydrous magnesium silicate two times
  5. customThe volatiles are evaporated in vacuo to a residue which
  6. dissolutionis dissolved in 25 ml of ethyl acetate
  7. filtrationfiltered
  8. temperatureThe filtrate is cooled

出典と根拠

ORDレコード
ord-ae1fc3543e1749939e12a883eca6fb18
出典データセット
uspto-grants-1998_02
特許番号
US05719278

反応ノート

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