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1-Hydroxybenzotriazole → [3-(2-Amino-3-methoxy-phenylcarbamoyl)-propyl]methyl-carbamic acid benzyl ester

HRID 1879356
ノート
印刷プレビュー

反応式

HRID 1879356 の反応式
[CH2:1]([O:8][C:9]([N:11]([CH3:18])[CH2:12][CH2:13][CH2:14][C:15]([OH:17])=O)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.C1C=CC2N(O)N=NC=2C=1.[CH3:38][O:39][C:40]1[CH:45]=[CH:44][CH:43]=[C:42]([NH2:46])[C:41]=1[NH2:47].C([O-])(O)=O.[Na+]>C1COCC1.C(Cl)CCl>[CH2:1]([O:8][C:9](=[O:10])[N:11]([CH2:12][CH2:13][CH2:14][C:15](=[O:17])[NH:46][C:42]1[CH:43]=[CH:44][CH:45]=[C:40]([O:39][CH3:38])[C:41]=1[NH2:47])[CH3:18])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 1842683-Methoxybenzene-1,2-diamineHCID 516892Sodium BicarbonateHCID 190283044-(((Benzyloxy)carbonyl)(methyl)amino)butanoic acid

生成物 1

HCID 67380324[3-(2-Amino-3-methoxy-phenylcarbamoyl)-propyl]methyl-carbamic acid benzyl ester

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 1.40 g 4-(benzyloxycarbonyl-methyl-amino)-butyric acid (obtained from 4-(methylamino)butyric acid and benzylchloroformate) in 25 mL THF were added 2.9 mL of DIPEA, 0.97 g of HOBt and 1.38 g EDC. After stirring for 5 min 0.80 g of 3-methoxy-benzene-1,2-diamine were added and the mixture was stirred for 3 h at rt. Sat. aq. NaHCO3 solution was added, the phases were separated and the organic phase was washed with brine. The combined organic phases were dried over MgSO4, and concentrated in vacuo.

後処理

  1. additionwere added
  2. customthe phases were separated
  3. washthe organic phase was washed with brine
  4. dry with materialThe combined organic phases were dried over MgSO4
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-86ec1af97acc4b8b9e965c4e7e863553
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08314253B2

反応ノート

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