HCID 135727397、化合物 → HCID 135727395、化合物

HRID 972436ノート

反応式

HRID 972436 の反応式
[CH2:1]([N:13]([CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH3:49])[S:14]([C:17]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:20]([OH:27])=[C:19]([N:28]=NC2C=CC(OC)=CC=2)[CH:18]=1)(=[O:16])=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[C:50]([NH:53][C:54]1[C:63]2[C:58](=[CH:59][CH:60]=[C:61]([N:65]=[N:66][C:67]3[CH:72]=[CH:71][CH:70]=[CH:69][C:68]=3[O:73][CH3:74])[C:62]=2[OH:64])[C:57]([S:75](Cl)(=[O:77])=[O:76])=[CH:56][CH:55]=1)(=[O:52])[CH3:51]>O1CCCC1>[C:50]([NH:53][C:54]1[C:63]2[C:58](=[CH:59][CH:60]=[C:61]([N:65]=[N:66][C:67]3[CH:72]=[CH:71][CH:70]=[CH:69][C:68]=3[O:73][CH3:74])[C:62]=2[OH:64])[C:57]([S:75]([NH:28][C:19]2[CH:18]=[C:17]([S:14](=[O:16])(=[O:15])[N:13]([CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH3:49])[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[C:20]=2[OH:27])(=[O:77])=[O:76])=[CH:56][CH:55]=1)(=[O:52])[CH3:51]

参加物

4

反応物 2

HCID 135727397HCID 135727397、化合物HCID 135755448HCID 135755448、化合物

生成物 1

HCID 135727395HCID 135727395、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran触媒

実験手順

A solution of 3.47 g (0.0050 mole) 4-(N,N-didodecylsulfamyl)-2-(p-methoxyphenylazo)-1-naphthol in 50 ml tetrahydrofuran containing 0.5 g 5% palladium/carbon catalyst was hydrogenated at low pressure and room temperature for 2 hr. The mixture was filtered and poured into water, then extracted with ether. The extract was concentrated to a gum which was dissolved in 50 ml pyridine. The solution was cooled in an ice bath, and 2.17 g (0.005 mole) 4-acetamido-5-hydroxy-6-(o-methoxyphenylazo)naphthalene-1-sulfonyl chloride was added. The mixture was stirred overnight at room temperature, then poured into ice-water containing 50 ml concentrated hydrochloric acid. The purple solid was recrystallized from dichloroethane and ethyl acetate to give, after drying under vacuum, an amorphous solid (Compound No. 14), m.p. 200°-202° C.

後処理

  1. filtrationThe mixture was filtered
  2. additionpoured into water
  3. extractionextracted with ether
  4. concentrationThe extract was concentrated to a gum which
  5. dissolutionwas dissolved in 50 ml pyridine
  6. temperatureThe solution was cooled in an ice bath
  7. customThe purple solid was recrystallized from dichloroethane and ethyl acetate
  8. customto give
  9. customafter drying under vacuum

出典と根拠

ORDレコード
ord-d42dbcc49ca24f05bf46f5d64fc73ed6
出典データセット
uspto-grants-1977_10
特許番号
US04053312

反応ノート

読み込み中…