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1-Hydroxybenzotriazole → [3-(2-Amino-4,5-dimethoxy-phenylcarbamoyl)-propyl]-methyl-carbamic acid benzyl ester

HRID 220239
ノート
印刷プレビュー

反応式

HRID 220239 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.Cl.Cl.[CH3:40][O:41][C:42]1[CH:43]=[C:44]([NH2:51])[C:45]([NH2:50])=[CH:46][C:47]=1[O:48][CH3:49].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:50][C:45]1[CH:46]=[C:47]([O:48][CH3:49])[C:42]([O:41][CH3:40])=[CH:43][C:44]=1[NH2:51])[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 516892Sodium BicarbonateHCID 130002194,5-Dimethoxybenzene-1,2-diamine--hydrogen chloride (1/2)HCID 190283044-(((Benzyloxy)carbonyl)(methyl)amino)butanoic acid

生成物 1

HCID 68414218
[3-(2-Amino-4,5-dimethoxy-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 0.95 g 4-(benzyloxycarbonyl-methyl-amino)-butyric acid in 20 mL THF were added 3.3 mL of DIPEA, 0.61 g of HOBt and 0.86 g EDC. After stirring for 5 min 1.0 g of 4,5-dimethoxy-benzene-1,2-diamine dihydrochloride was added and the mixture was stirred at rt overnight. Saturated 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. additionwas 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-22ca4ff8a7674726a83415621108f133
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08202885B2

反応ノート

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