1,4-Dioxane hydrochloride → HCID 59622872、化合物

HRID 517664ノート

反応式

HRID 517664 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]([CH2:18][CH2:19][N:20]2[CH2:28][CH2:27][N:26]([CH2:29][C:30](=[O:36])[O:31]C(C)(C)C)[CH2:25][CH2:24][N:23]([CH2:37][C:38]([O:40]C(C)(C)C)=[O:39])[CH2:22][CH2:21]2)[CH2:10][C:11]([O:13]C(C)(C)C)=[O:12])=[CH:4][CH:3]=1.Cl.O1CCOCC1>C(OCC)C>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][N:9]([CH2:18][CH2:19][N:20]2[CH2:21][CH2:22][N:23]([CH2:37][C:38]([OH:40])=[O:39])[CH2:24][CH2:25][N:26]([CH2:29][C:30]([OH:36])=[O:31])[CH2:27][CH2:28]2)[CH2:10][C:11]([OH:13])=[O:12])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 59622792Tert-butyl 2-{[(4-aminophenyl)methyl](2-{4,7-bis[2-(tert-butoxy)-2-oxoethyl]-1,4,7-triazonan-1-yl}ethyl)amino}acetate

生成物 1

HCID 59622872HCID 59622872、化合物収率 119.7%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To Compound 9 (39 mg, 62.9 μmol) with an ice cooling bath around was added 6 mL of 4 M HCl/dioxane dropwise. After the addition was complete, the reaction mixture was gradually warmed to room temperature and allowed to stir overnight at room temperature. After completion 50 mL of ethyl ether was added to the reaction mixture with vigorous stirring and the resulting slurry was kept in the freezer for 2 h. The precipitate was collected and washed with ethyl ether, then immediately lyophilized with water and evaporated to provide pure salt as light yellow solid Compound 10 (34 mg, 85%). NMR (D2O, 300 MHz) δ 2.97 (m, 4H), 3.21 (m, 6H), 3.33 (s, 4H), 3.48 (t, J=5.4 Hz, 2H), 3.93 (s, 4H), 3.99 (s, 2H), 4.46 (s, 2H), 7.40 (d, J=6.4 Hz, 2H), 7.59 (d, J=6.4 Hz, 2H).

後処理

  1. additionAfter the addition
  2. stirringwith vigorous stirring
  3. waitthe resulting slurry was kept in the freezer for 2 h
  4. customThe precipitate was collected
  5. washwashed with ethyl ether
  6. customevaporated

出典と根拠

ORDレコード
ord-757c13486a524676832e5bbd7a82d48c
出典データセット
uspto-grants-2015_08
特許番号
US09115094B2

反応ノート

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