Sodium cyanoborohydride → HCID 54173271、化合物

HRID 260546ノート

反応式

HRID 260546 の反応式
[NH2:1][CH:2]([C:6]#[N:7])[C:3]([OH:5])=[O:4].[CH3:8][C:9]1C=CC(S(OCC)(=O)=O)=CC=1.[CH3:21][N:22]([CH:24]=[N:25][S:26]([C:29]1[C:30]([C:35]2[CH:40]=[CH:39][C:38]([CH:41]=O)=[CH:37][CH:36]=2)=[CH:31][CH:32]=[CH:33][CH:34]=1)(=[O:28])=[O:27])[CH3:23].C([BH3-])#N.[Na+]>ClCCl>[C:6]([CH:2]([NH:1][CH2:41][C:38]1[CH:39]=[CH:40][C:35]([C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][C:29]=2[S:26]([N:25]=[CH:24][N:22]([CH3:23])[CH3:21])(=[O:28])=[O:27])=[CH:36][CH:37]=1)[C:3]([O:5][CH2:8][CH3:9])=[O:4])#[N:7]

参加物

5

反応物 3

HCID 5003444Sodium cyanoborohydrideHCID 54273713N'-(4'-Formyl[1,1'-biphenyl]-2-sulfonyl)-N,N-dimethylmethanimidamideHCID 86749579HCID 86749579、化合物

生成物 1

HCID 54173271HCID 54173271、化合物収率 29.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2 g of ethyl mono (4-methylbenzenesulfonate) aminocyano acetate of Stage B of Example 1 and 1.9 g of N-[(dimethylamino) methylene]-4'-formyl-(1,1'-biphenyl)-2-sulfonamide of Stage A of Example 1 were stirred in dichloromethane at 35° for 3 hours and then 0.396 g of sodium cyano borohydride were added. The solution was stirred at ambient temperature for 18 hours and the reaction mixture was filtered, washed with water and evaporated. After chromatography on silica (dichloromethane-ethyl acetate 85-15), 770 mg of the expected product were obtained, identical to that of Stage C of Example 1.

後処理

  1. filtrationthe reaction mixture was filtered
  2. washwashed with water
  3. customevaporated

出典と根拠

ORDレコード
ord-103d0109561a4abead21deeda985d7ac
出典データセット
uspto-grants-1996_06
特許番号
US05527919

反応ノート

読み込み中…