Hydrochloric Acid → 3-Cyclopentyloxy-4-methoxyphenyldiazonium tetrafluoroborate

HRID 356959

반응식

HRID 356959 반응식
Cl.[CH:2]1([O:7][C:8]2[CH:9]=[C:10]([CH:12]=[CH:13][C:14]=2[O:15][CH3:16])[NH2:11])[CH2:6][CH2:5][CH2:4][CH2:3]1.[N:17]([O-])=O.[Na+].[F:21][B-:22]([F:25])([F:24])[F:23].[Na+]>O>[F:21][B-:22]([F:25])([F:24])[F:23].[CH:2]1([O:7][C:8]2[CH:9]=[C:10]([N+:11]#[N:17])[CH:12]=[CH:13][C:14]=2[O:15][CH3:16])[CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 27793343-(Cyclopentyloxy)-4-methoxyanilineHCID 4343483Sodium TetrafluoroborateHCID 23668193Sodium Nitrite

생성물 1

HCID 114722533-Cyclopentyloxy-4-methoxyphenyldiazonium tetrafluoroborate수율 101.2%

시약·촉매·용매 1

HCID 962Water용매3회

실험 절차

A stirred solution of concentrated hydrochloric acid (1.7 mL) in water (5 mL) from 0° C. and 5° C. is treated with 3-cyclopentyloxy-4-methoxyaniline (0.83 g), followed by a solution of sodium nitrite (0.29 g) in water (0.6 mL), at such a rate that the temperature remains from 0° C. and 5° C. The resulting solution is stirred for a further 10 minutes, while keeping the temperature below 5° C. The stirred solution, while still maintained at below 5° C., is then treated dropwise with a solution of sodium tetrafluoroborate (0.88 g) in water (1.8 mL). The resulting precipitate is filtered off, washed with cold water (3 mL) and dried in vacuo, to give 3-cyclopentyloxy-4-methoxyphenyldiazonium tetrafluoroborate (1.24 g) in the form of a gray solid, m.p. 120° C.

후처리

  1. customremains from 0° C. and 5° C
  2. customthe temperature below 5° C
  3. temperatureThe stirred solution, while still maintained at below 5° C.
  4. filtrationThe resulting precipitate is filtered off
  5. washwashed with cold water (3 mL)
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-0d965eeb365e4452a161846ad65091c6
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840724

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