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Formaldehyde → 1-Methyl-4-({1-[(6-methylpyridin-3-yl)carbonyl]azetidin-3-yl}carbonyl)-1,4-diazepane

HRID 1402759
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HRID 1402759 반응식
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[CH2:13][CH:12]([C:14]([N:16]3[CH2:22][CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)=[O:15])[CH2:11]2)=[O:9])=[CH:4][CH:3]=1.[CH2:23]=O>C(O)=O>[CH3:23][N:19]1[CH2:20][CH2:21][CH2:22][N:16]([C:14]([CH:12]2[CH2:13][N:10]([C:8]([C:5]3[CH:6]=[N:7][C:2]([CH3:1])=[CH:3][CH:4]=3)=[O:9])[CH2:11]2)=[O:15])[CH2:17][CH2:18]1
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참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 667401031-({1-[(6-Methylpyridin-3-yl)carbonyl]azetidin-3-yl}carbonyl)-1,4-diazepane

생성물 1

HCID 667398581-Methyl-4-({1-[(6-methylpyridin-3-yl)carbonyl]azetidin-3-yl}carbonyl)-1,4-diazepane수율 75%

시약·촉매·용매 1

HCID 284Formic Acid용매

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온도
100 °C

실험 절차

To a stirred solution of 1-({1-[(6-methylpyridin-3-yl)carbonyl]azetidin-3-yl}carbonyl)-1,4-diazepane (50 mg, 0.162 mmol) in formic acid (0.25 mL) was added formaldehyde (37% aq. sol., 0.097 mL, 1.296 mmol) and the reaction mixture was heated at 100° C. for 5 hours. Volatiles were then removed at reduced pressure to give the title compound (38 mg, 75%) after purification by silica FCC (eluting with 95:4.5:0.5 to 92.5:7.25:0.75 gradient of DCM/MeOH/NH3).

후처리

  1. customVolatiles were then removed at reduced pressure

출처 및 근거

ORD 기록
ord-1ea161591db04d1ca9f7ede124aab07a
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08912176B2

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