1,4-Dioxane hydrochloride → HCID 59622872, 화합물

HRID 517664노트

반응식

HRID 517664 반응식
[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

참가 물질

4

반응물 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

생성물 1

HCID 59622872HCID 59622872, 화합물수율 119.7%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-757c13486a524676832e5bbd7a82d48c
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115094B2

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