Sodium borohydride → HCID 55036, 화합물

HRID 2417617노트

반응식

HRID 2417617 반응식
[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

참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 13298561HCID 13298561, 화합물

생성물 1

HCID 55036HCID 55036, 화합물수율 99.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-c7fb2629372847f18e853da843972340
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04469695

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