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Ammonia → HCID 69330037、化合物

HRID 2299621
ノート
印刷プレビュー

反応式

HRID 2299621 の反応式
[OH:1][C:2]1[CH:38]=[CH:37][C:5]2[CH2:6][CH2:7][CH2:8][CH:9]([N:11]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:12][C@H:13]([O:22][Si:23]([CH2:28][CH3:29])([CH2:26][CH3:27])[CH2:24][CH3:25])[CH2:14][O:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:10][C:4]=2[CH:3]=1.[N:39]1[CH:44]=CC=CC=1.ClC(OC1C=CC([N+]([O-])=O)=CC=1)=[O:47].N>ClCCl.CN(C)C1C=CN=CC=1.C(O)C.O>[O:15]([CH2:14][C@@H:13]([O:22][Si:23]([CH2:26][CH3:27])([CH2:24][CH3:25])[CH2:28][CH3:29])[CH2:12][N:11]([C:30]([O:32][C:33]([CH3:35])([CH3:34])[CH3:36])=[O:31])[CH:9]1[CH2:8][CH2:7][CH2:6][C:5]2[CH:37]=[CH:38][C:2]([O:1][C:44](=[O:47])[NH2:39])=[CH:3][C:4]=2[CH2:10]1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 222AmmoniaHCID 1049PyridineHCID 821294-Nitrophenyl chloroformateHCID 57157362HCID 57157362、化合物

生成物 1

HCID 69330037HCID 69330037、化合物

試薬・触媒・溶媒 4

HCID 142844-(Dimethylamino)pyridine触媒
HCID 702
Ethanol
溶媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒

実験手順

Under nitrogen, to a solution of N-(3-hydroxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)-N-[(2S)-3-phenoxy-2-(triethylsilyloxy)propyl]-tert-butoxycarbonylamine (150 mg) in dichloromethane (5 ml) were added pyridine (64 ml), 4-nitrophenyl chloroformate (116 mg) and a catalytic amount of 4-dimethylaminopyridine at 5° C. After being stirred at the same temperature for 2 hours, to this one was added about 6.8M ammonia in ethanol (0.5 ml), and the mixture was stirred at room temperature for 12 hours. The resulting mixture was pured into water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1) to give N-[(2S)-3-phenoxy-2-(triethyl-silyloxy)propyl]-N-[3-carbamoyloxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl]-tert-butoxycarbonylamine (129 mg).

後処理

  1. customat 5° C
  2. stirringthe mixture was stirred at room temperature for 12 hours
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-4e96b4e991bc4d8dbf6ed6f88a55dcf6
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06495546B1

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