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4,4,5,5,6,6,7,7,7-Nonafluoroheptanenitrile → HCID 22013473、化合物

HRID 1005497
ノート
印刷プレビュー

反応式

HRID 1005497 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

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

生成物 1

HCID 22013473HCID 22013473、化合物収率 13.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-866895660b7147d3ad3492cec1773528
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06054615

反応ノート

読み込み中…

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