Potassium Hydroxide → HCID 18367242、化合物

HRID 380150

反応式

HRID 380150 の反応式
[Si:1]([O:18][C:19]1[CH:28]=[CH:27][CH:26]=[C:25]2[C:20]=1[CH2:21][CH2:22][CH2:23][CH:24]2[NH2:29])([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:30][C:31]1[CH:36]=[CH:35][C:34]([C:37]2[N:38]=[C:39]([C:49](=O)[CH2:50][CH2:51][CH:52]=O)[O:40][C:41]=2[C:42]2[CH:47]=[CH:46][C:45]([CH3:48])=[CH:44][CH:43]=2)=[CH:33][CH:32]=1.[BH3-]C#N.[Na+].[OH-].[K+]>C(O)(=O)C.CO>[CH3:30][C:31]1[CH:32]=[CH:33][C:34]([C:37]2[N:38]=[C:39]([CH:49]3[CH2:50][CH2:51][CH2:52][N:29]3[CH:24]3[C:25]4[C:20](=[C:19]([O:18][Si:1]([C:14]([CH3:16])([CH3:17])[CH3:15])([C:8]5[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=5)[C:2]5[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=5)[CH:28]=[CH:27][CH:26]=4)[CH2:21][CH2:22][CH2:23]3)[O:40][C:41]=2[C:42]2[CH:47]=[CH:46][C:45]([CH3:48])=[CH:44][CH:43]=2)=[CH:35][CH:36]=1

参加物

7

反応物 4

HCID 14797Potassium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 18367231HCID 18367231、化合物HCID 183673471-[4,5-Bis(4-methylphenyl)oxazol-2-yl)butan-1,4-dione

生成物 1

HCID 18367242HCID 18367242、化合物収率 94.8%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒

実験手順

A solution of 1,2,3,4-tetrahydro-5-t-butyldiphenylsilyloxy-1-naphthaleneamine (0.21 g), 1-[4,5-bis(4-methylphenyl)oxazol-2-yl)butan-1,4-dione (0.12 g), NaBH3CN (84 mg) and KOH (30 mg) in acetic acid (0.5 ml) and methanol (4 ml). After being stirred for 3 days at room temperature, the solvent was evaporated in vacuo. The residue was partitioned between ethyl acetate and sat. NaHCO3. The organic layer was washed with brine. The dried solvent was evaporated in vacuo. The residue was purified by chromatography on silica gel to give 1-[2-[4,5-bis(4-methylphenyl)oxazol-2-yl]pyrrolidin-1-yl]-1,2,3,4-tetrahydro-5-t-butyldiphenylsilyloxynaphthalene (0.24 g).

後処理

  1. customthe solvent was evaporated in vacuo
  2. customThe residue was partitioned between ethyl acetate and sat. NaHCO3
  3. washThe organic layer was washed with brine
  4. customThe dried solvent was evaporated in vacuo
  5. customThe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-4c38a542bedc46a9aa615bb3bdf6f9bb
出典データセット
uspto-grants-2001_10
特許番号
US06300344B1

関連ノート

読み込み中…