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N,N'-Bis(tert-butoxycarbonyl)-1H-pyrazole-1-carboxamidine → HCID 178426314、化合物

HRID 251223
ノート
印刷プレビュー

反応式

HRID 251223 の反応式
[CH3:1][C:2]1[C:3]([N:8]([CH:13]2[C:22]3[N:21]=[CH:20][CH:19]=[CH:18][C:17]=3[CH2:16][CH2:15][CH2:14]2)[CH2:9][CH2:10][CH2:11][NH2:12])=[N:4][CH:5]=[CH:6][CH:7]=1.C(OC(=O)[NH:29][C:30](=NC(OC(C)(C)C)=O)[N:31]1C=CC=N1)(C)(C)C.C(OC(=O)NC(CCCN(CC1C(C)=CC=CN=1)C1C2N=CC=CC=2CCC1)=NC(OC(C)(C)C)=O)(C)(C)C>C1COCC1>[CH3:1][C:2]1[C:3]([N:8]([CH:13]2[C:22]3[N:21]=[CH:20][CH:19]=[CH:18][C:17]=3[CH2:16][CH2:15][CH2:14]2)[CH2:9][CH2:10][CH2:11][NH:12][C:30]([NH2:31])=[NH:29])=[N: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

5

反応物 3

HCID 4428040N,N'-Bis(tert-butoxycarbonyl)-1H-pyrazole-1-carboxamidineHCID 67271945N1-(3-methyl-pyridin-2-yl)-N-(5,6,7,8-tetrahydro-quinolin-8-yl)-propane-1,3-diamineHCID 86623813({3-[(3-Methyl-pyridin-2-ylmethyl)-(5,6,7,8-tetrahydro-quinolin-8-yl)-amino]-propyl}-tert-butoxycarbonylimino-methyl)-carbamic acid tert butyl ester

生成物 1

HCID 178426314HCID 178426314、化合物

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

N1-(3-methyl-pyridin-2-yl)-N1-(5,6,7,8-tetrahydro-quinolin-8-yl)-propane-1,3-diamine (63 mg, 0.20 mmol) and (tert-butoxycarbonylimino-pyrazol-1-yl-methyl)-carbamic acid tert-butyl ester (110 mg, 0.31 mmol) was stirred in THF (0.3 mL) for 16 hours. The solvent was removed under reduced pressure, CH2Cl2 (10 mL) was added and the organic phase washed with 15% aqueous NaOH solution (5×5 mL). The organic phase was then dried (Na2SO4) and concentrated under reduced pressure to afford, after column chromatography with silica gel (33:1:0.1 CH2Cl2/MeOH:NH4OH), ({3-[(3-methyl-pyridin-2-ylmethyl)-(5,6,7,8-tetrahydro-quinolin-8-yl)-amino]-propyl}-tert-butoxycarbonylimino-methyl)-carbamic acid tert butyl ester as a pale brown sticky solid (50 mg, 49%),

後処理

  1. customThe solvent was removed under reduced pressure, CH2Cl2 (10 mL)
  2. additionwas added
  3. washthe organic phase washed with 15% aqueous NaOH solution (5×5 mL)
  4. dry with materialThe organic phase was then dried (Na2SO4)
  5. concentrationconcentrated under reduced pressure
  6. customto afford

出典と根拠

ORDレコード
ord-6fc04c43209e4b12b8841c4a5fac2a48
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07863293B2

反応ノート

読み込み中…

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