Sodium borohydride → HCID 55036、化合物

HRID 2417617ノート

反応式

HRID 2417617 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11](=[O:27])[CH2:12][N:13]2[CH2:18][CH2:17][N:16]([C:19]3[C:20](=[O:26])[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)[CH2:15][CH2:14]2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[BH4-].[Na+]>CO.C(Cl)(Cl)Cl>[OH:27][CH:11]([C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)[CH2:12][N:13]1[CH2:18][CH2:17][N:16]([C:19]2[C:20](=[O:26])[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH2:15][CH2:14]1

参加物

5

反応物 2

HCID 4311764Sodium borohydrideHCID 13298561HCID 13298561、化合物

生成物 1

HCID 55036HCID 55036、化合物収率 99.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

実験手順

To a solution of 2-[4-[2-(3,4-dimethoxyphenyl)-2-oxoethyl]-1-piperazinyl]-2,4,6-cycloheptatrien-1-one (1.33 g, described above) in methanol (20 ml) and chloroform (5 ml), sodium borohydride (0.31 g) was added portionwise over a period of one hr. The solvent was then removed under vacuum. The residue was taken up in chloroform, washed with water, ammonium chloride solution followed by water, dried and evaporated to give the title compound (1.33 g): mp 122°-124° C.; ir(CHCl3) 3420, 1565, 1260 and 1140 cm-1 ; uv max(MeOH) 352 (ε=10040), 256 (ε=15660) and 227 nm (ε=20250); nmr(CDCl3) δ2.6 (m, 6H), 3.3 (m, 4H), 3.85 (s, 6H), 4.7 (m,1H) and 6.8 (m,6H); and Anal. Calcd for C21H26N2O4 : C, 68.08% H, 7.08% N, 7.56% and Found: C, 67.78% H, 7.06% N, 7.36%.

後処理

  1. customThe solvent was then removed under vacuum
  2. washwashed with water, ammonium chloride solution
  3. customdried
  4. customevaporated

出典と根拠

ORDレコード
ord-c7fb2629372847f18e853da843972340
出典データセット
uspto-grants-1984_09
特許番号
US04469695

反応ノート

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