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1-Hydroxybenzotriazole → HCID 22461188、化合物

HRID 1937445
ノート
印刷プレビュー

反応式

HRID 1937445 の反応式
[C:1]([C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=O)=[C:7]([O:14][CH3:15])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl.C(N=C=NCCCN(C)C)C.ON1C2C=CC=CC=2N=N1.[NH2:38][C:39]1[CH:40]=[C:41]([CH:45]2[CH2:49][CH2:48][CH2:47][N:46]2[C:50]([O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[O:51])[CH:42]=[CH:43][CH:44]=1>CN(C=O)C.O>[C:1]([C:5]1[CH:13]=[CH:12][C:8]([C:9]([NH:38][C:39]2[CH:40]=[C:41]([CH:45]3[CH2:49][CH2:48][CH2:47][N:46]3[C:50]([O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[O:51])[CH:42]=[CH:43][CH:44]=2)=[O:11])=[C:7]([O:14][CH3:15])[CH:6]=1)([CH3:2])([CH3:3])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 126137394-tert-Butyl-2-methoxybenzoic acidHCID 22461189HCID 22461189、化合物

生成物 1

HCID 22461188HCID 22461188、化合物収率 34.8%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-tert-butyl-2-methoxy-benzoic acid (0.05 g) in DMF (1.5 mL) at room temperature, was added in order, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (0.046 g), 1-hydroxy-benzotriazole (0.033 g) and 15 min. later, (±)-2-(3-aminophenyl)-1-(tert-butyloxycarbonyl)-pyrrolidine (0.05 g). The reaction mixture was allowed to stir for 17 h and then poured into water. The aqueous mixture was extracted with ethyl acetate twice. The combined organic layer was washed with brine, dried (sodium sulfate) and evaporated in vacuo to afford an amber oil. Suction silica gel chromatography eluting with ethyl acetate in hexane (from 30% to 100%, in 10% increments) gave desired product as an amber solid (0.03 g).

後処理

  1. extractionThe aqueous mixture was extracted with ethyl acetate twice
  2. washThe combined organic layer was washed with brine
  3. dry with materialdried (sodium sulfate)
  4. customevaporated in vacuo
  5. customto afford an amber oil
  6. washSuction silica gel chromatography eluting with ethyl acetate in hexane (from 30% to 100%, in 10% increments)

出典と根拠

ORDレコード
ord-2a7448754bd9482087dcd591c53efaba
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06395759B1

反応ノート

読み込み中…

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