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 863024노트

반응식

HRID 863024 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ae1fc3543e1749939e12a883eca6fb18
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05719278

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