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Tetrahydrofuran → Bis(1-octyloxy-2,2,6,6-tetramethylpiperidin-4-yl) Hydrazine-1,2-dicarboxylate

HRID 742614
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HRID 742614 반응식
ClC(Cl)(O[C:5](=[O:11])[O:6][C:7](Cl)(Cl)Cl)Cl.[CH2:13]([O:21][N:22]1[C:27]([CH3:29])([CH3:28])[CH2:26][CH:25]([OH:30])[CH2:24][C:23]1([CH3:32])[CH3:31])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20].O.[NH2:34][NH2:35].[C:36](=[O:39])([O-])[O-].[Na+].[Na+].[O:42]1[CH2:46][CH2:45][CH2:44][CH2:43]1>O.C(N(CC)CC)C>[NH:34]([C:5]([O:6][CH:7]1[CH2:26][C:27]([CH3:29])([CH3:28])[N:22]([O:42][CH2:46][CH2:45][CH2:44][CH2:43][CH2:13][CH2:14][CH2:15][CH3:16])[C:23]([CH3:31])([CH3:32])[CH2:24]1)=[O:11])[NH:35][C:36]([O:30][CH:25]1[CH2:26][C:27]([CH3:29])([CH3:28])[N:22]([O:21][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[C:23]([CH3:31])([CH3:32])[CH2:24]1)=[O:39]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 8028Tetrahydrofuran2회HCID 10340Sodium CarbonateHCID 24654Hydrazine hydrate (1:1)HCID 94429TriphosgeneHCID 113466831-Octyloxy-2,2,6,6-tetramethylpiperidin-4-ol

생성물 1

HCID 15345986Bis(1-octyloxy-2,2,6,6-tetramethylpiperidin-4-yl) Hydrazine-1,2-dicarboxylate

시약·촉매·용매 2

HCID 962Water용매HCID 8471Triethylamine용매

실험 절차

To a solution of 29.7 g of triphosgene in 120 mL of tetrahydrofuran (THF) is added a solution of 85.7 g of 1-octyloxy-2,2,6,6-tetramethylpiperidin-4-ol and 42.0 mL of triethylamine in 240 mL of THF over 4 hours at 5°-10° C., followed by 7.3 mL of hydrazine hydrate. After stirring the reaction mixture at room temperature for 18 hours, a solution of 71.0 g of sodium carbonate in 500 mL of water is added and the organic layer is removed, washed with water and dried over anhydrous magnesium sulfate. The dried solution is evaporated to afford 97.2 g of the title compound as an oil.

후처리

  1. customthe organic layer is removed
  2. washwashed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe dried solution is evaporated

출처 및 근거

ORD 기록
ord-d5829c5eeb77472e9e7b62e4e6b15504
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05554754

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