Tempo → 4,8-Dioxa-3H-perfluorononanoic acid

HRID 2407650

반응식

HRID 2407650 반응식
CC1(C)N([O])C(C)(C)CCC1.CC(O[Na])=[O:14].[F:17][C:18]([F:38])([CH:21]([F:37])[O:22][C:23]([F:36])([F:35])[C:24]([F:34])([F:33])[C:25]([F:32])([F:31])[O:26][C:27]([F:30])([F:29])[F:28])[CH2:19][OH:20]>O.O.O.O.[N+]([O-])([O-])=O.[Mn+2].[N+]([O-])([O-])=O.O.O.O.O.O.O.[N+]([O-])([O-])=O.[Co+2].[N+]([O-])([O-])=O.C(O)(=O)C>[F:17][C:18]([F:38])([CH:21]([F:37])[O:22][C:23]([F:36])([F:35])[C:24]([F:33])([F:34])[C:25]([F:31])([F:32])[O:26][C:27]([F:28])([F:29])[F:30])[C:19]([OH:14])=[O:20]

참가 물질

7

반응물 3

HCID 2724126TempoHCID 866682301-Propanol, 2,2,3-trifluoro-3-[1,1,2,2,3,3-hexafluoro-3-(trifluoromethoxy)propoxy]-HCID 178418247HCID 178418247, 화합물

생성물 1

HCID 529152994,8-Dioxa-3H-perfluorononanoic acid수율 70.6%

시약·촉매·용매 3

HCID 24821Cobaltous nitrate hexahydrate촉매HCID 182616Manganese nitrate tetrahydrate촉매HCID 176Acetic Acid용매

실험 절차

50 mL of acetic acid, 0.137 g of manganese nitrate tetrahydrate, 0.159 g of cobalt nitrate hexahydrate, TEMPO (0.42 g), CH3CO2Na (2.24 g) and 10 g of 2,2,3-trifluoro-3-(1,1,2,2,3,3-hexafluoro-3-trifluoromethoxy-propoxy)-propan-1-ol were placed in a reaction vessel as described in example 17 except that a 100 mL vessel instead of a 200 mL vessel was used. The reaction was carried out and worked up as described in example 9. Distillation gave 7.29 g of acid (1.6 mmHg, 58° C.). Yield: 70%.

후처리

  1. customas described in example 17 except that a 100 mL vessel instead of a 200 mL vessel
  2. distillationDistillation

출처 및 근거

ORD 기록
ord-516ce911e58946cf9feb52b0e052555f
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809580B2

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