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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 503192、化合物

HRID 977301
ノート
印刷プレビュー

反応式

HRID 977301 の反応式
[C:1]([NH:5][C:6]([C@@H:8]1[CH2:13][C@H:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:11][CH2:10][N:9]1[CH2:20][C@@H:21]([OH:41])[C@@H:22]([NH:30]C(OCC1C=CC=CC=1)=O)[CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Li].[N:43]1[CH:48]=[CH:47][CH:46]=[CH:45][C:44]=1[CH2:49][O:50][C:51]([NH:53][C@H:54]([C:59]([OH:61])=O)[C@H:55]([CH2:57][CH3:58])[CH3:56])=[O:52].ON1C2C=CC=CC=2N=N1.C(N=C=NCCCN(C)C)C>CN(C=O)C.CCOCC.[Pd].CO>[C:1]([NH:5][C:6]([C@@H:8]1[CH2:13][C@H:12]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:11][CH2:10][N:9]1[CH2:20][C@@H:21]([OH:41])[C@@H:22]([NH2:30])[CH2:23][C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3].[C:1]([NH:5][C:6]([C@@H:8]1[CH2:13][C@H:12]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:11][CH2:10][N:9]1[CH2:20][C@@H:21]([OH:41])[C@@H:22]([NH:30][C:59](=[O:61])[C@H:54]([C@H:55]([CH2:57][CH3:58])[CH3:56])[NH:53][C:51]([O:50][CH2:49][C:44]1[CH:45]=[CH:46][CH:47]=[CH:48][N:43]=1)=[O:52])[CH2:23][C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 503167HCID 503167、化合物HCID 3028194LithiumHCID 54304856HCID 54304856、化合物

生成物 2

HCID 503192HCID 503192、化合物収率 161.8%
HCID 22870891
HCID 22870891、化合物

試薬・触媒・溶媒 4

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

N-tert-butyl-1-{3(S)-amino-2(R)-hydroxy-4-phenylbutyl}-4(R)-phenylpiperidine-2(S)-carboxamide {prepared by hydrogenolysis (5% Pd/C, 1 atmosphere, MeOH, 2 h) from 0.605 mg (0.108 mmol) of N-tert-butyl-1-{3(S)-(benzyloxycarbonylamino)-2(R)-hydroxy-4-phenylbutyl}-4(R)-phenylpiperidine-2(S)-carboxamide (see entry 1 of Table I)} was dissolved in DMF (1.6 mL). The lithium salt of N-{(2-pyridinylmethoxy)carbonyl}isoleucine (586 mg, 0.228 mmol), 1-hydroxybenzotriazole (32 mg, 0.237 mmol) and N-ethyl-N'-{3-(dimethylamino)propyl}carbodiimide (45.4 mg, 0,237 mmol) were added to the solution. The mixture was stirred at room temperature for 18 h. Thereafter, the reaction mixture was diluted with Et2O, washed with H2O, a saturated aqueous solution of NaHCO3 (2×) and brine, dried (MgSO4) and evaporated to dryness. The resulting yellow oil was purified by flash chromatography (SiO2, eluent: CHCl3, MeOH, 97.5:2.5 and then 95:5) to give the title compound as a white solid (58.7 mg). FAB mass spectrum, m/z: 672 (M+H)+.

後処理

  1. washwashed with H2O
  2. dry with materiala saturated aqueous solution of NaHCO3 (2×) and brine, dried (MgSO4)
  3. customevaporated to dryness
  4. customThe resulting yellow oil was purified by flash chromatography (SiO2, eluent

出典と根拠

ORDレコード
ord-2b0d3b9e2c03479d8b26c9a25ab2512b
出典データセット
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05614533

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート