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4,4,5,5,6,6,7,7,7-Nonafluoroheptanenitrile → HCID 22013473, 화합물

HRID 1005497
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HRID 1005497 반응식
[C:1]([CH2:14][CH2:15][C:16]#[N:17])([C:4]([C:7]([C:10]([F:13])([F:12])[F:11])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2]>C1COCC1>[F:2][C:1]([F:3])([C:4]([F:5])([F:6])[C:7]([F:8])([F:9])[C:10]([F:11])([F:12])[F:13])[CH2:14][CH2:15][CH2:16][NH2:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 145126814,4,5,5,6,6,7,7,7-Nonafluoroheptanenitrile

생성물 1

HCID 22013473HCID 22013473, 화합물수율 13.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
110 °C

실험 절차

A 210-ml shaker tube was charged with 30 g of C4F9CH2CH2CN, 4.0 g of PtB on activated carbon (2%) and 30 ml THF. The vessel was closed, cooled, evacuated and pressured with hydrogen to 3.5 MPa. The vessel was heated to 110° C. and hydrogen pressure was adjusted to 10.3 MPa. The mixture was shaken for 16 h. The vessel was cooled and the gas was vented slowly. The contents were filtered and the filtrate was distilled to remove THF. The residue was distilled at reduced pressure to give 4,4,5,5,6,6,7,7,7-nonafluoroheptylamine (4.0 g, 13%, b.p. 94-97° C./24 kPa absolute) and di(4,4,5,5,6,6,7,7,7-nonailuoroheptyl)amine (20.5 g, 69%, b.p. 105-108° C./270 Pa absolute). The distillation residue (0.2 g) was mainly (C4F9CH2CH2CH2)3N.

후처리

  1. customThe vessel was closed
  2. temperaturecooled
  3. customevacuated
  4. temperatureThe vessel was cooled
  5. filtrationThe contents were filtered
  6. distillationthe filtrate was distilled
  7. customto remove THF
  8. distillationThe residue was distilled at reduced pressure

출처 및 근거

ORD 기록
ord-866895660b7147d3ad3492cec1773528
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06054615

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