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Hydrazoic acid → 5-(chloromethyl)-1-cyclohexyl-1H-1,2,3,4-tetrazole

HRID 1277419
ノート
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反応式

HRID 1277419 の反応式
[Cl:1][CH2:2][C:3]([NH:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1)=O.P(Cl)(Cl)(Cl)(Cl)Cl.[NH:18]=[N+:19]=[N-:20]>C1C=CC=CC=1>[CH:6]1([N:5]2[C:3]([CH2:2][Cl:1])=[N:20][N:19]=[N:18]2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24530Hydrazoic acidHCID 24819Phosphorus pentachlorideHCID 2223652-Chloro-N-cyclohexylacetamide

生成物 1

HCID 130202245-(chloromethyl)-1-cyclohexyl-1H-1,2,3,4-tetrazole

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

Into 150 ml of dried benzene, 17.6 g of N-chloroacetylcyclohexylamine was added. While the inside temperature is kept below 15° C. by ice-cooling the outside of the reaction vessel, 24 g of phosphorus pentachloride (PCl5) was added under stirring condition. After completion of the addition, the stirring is continued for 2 hours at a room temperature, then the reaction mixture is concentrated to a half volume thereof by using an evaporator with a bath temperature of below 50° C. To the concentrated reaction mixture was added dropwise 100 ml of benzene containing 10% of HN3 under stirring condition for 90 minutes while keeping the inside temperature below 15° C. After the addition operation, the reaction mixture is allowed to stand overnight. Then the reaction mixture is refluxed for 3 hours with stirring. The thus obtained concentrate is extracted with 200 ml of chloroform. The chloroform layer is washed with water, 5% NaHCO3 aqueous solution, 5% hydrochloric acid and water in this order and dried with Na2SO4. After removal of the drying agent by filtration, the mother liquour is concentrated and the residue thus obtained is recrystallized from chloroform-petroleum ether to obtain 16.1 g of 1-cyclohexyl-5-chloromethyltetrazol in the form of colorless needle like crystals. Melting point: 101° to 103.5° C.

後処理

  1. customis kept below 15° C. by ice-
  2. additionwas added
  3. additionAfter completion of the addition
  4. concentrationthe reaction mixture is concentrated to a half volume
  5. customan evaporator with a bath temperature of below 50° C
  6. customTo the concentrated reaction mixture
  7. stirringunder stirring condition for 90 minutes
  8. customthe inside temperature below 15° C
  9. waitto stand overnight
  10. temperatureThen the reaction mixture is refluxed for 3 hours
  11. stirringwith stirring
  12. customThe thus obtained
  13. concentrationconcentrate
  14. extractionis extracted with 200 ml of chloroform
  15. washThe chloroform layer is washed with water, 5% NaHCO3 aqueous solution, 5% hydrochloric acid and water in this order
  16. dry with materialdried with Na2SO4
  17. customAfter removal of the drying agent
  18. filtrationby filtration
  19. concentrationthe mother liquour is concentrated
  20. customthe residue thus obtained
  21. customis recrystallized from chloroform-petroleum ether

出典と根拠

ORDレコード
ord-e292b5a48aaa4521b4f883103049e2c7
出典データセット
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04277479

反応ノート

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