Tetraethylammonium Hydroxide → HCID 23509207, 화합물

HRID 870114

반응식

HRID 870114 반응식
I[C:2]1[CH:3]=[C:4]([C:8]2[C:20]3[NH:19][C:18]4[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=4)[C:12]=3[CH:11]=[CH:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1.[OH-].C([N+]([CH2:29][CH3:30])(CC)CC)C>CC(C)=O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:30]1([C:9]2[CH:10]=[CH:11][C:12]3[C:13]4[C:18](=[CH:17][CH:16]=[CH:15][CH:14]=4)[NH:19][C:20]=3[C:8]=2[C:4]2[CH:3]=[CH:2][CH:7]=[CH:6][CH:5]=2)[CH:29]=[CH:6][CH:7]=[CH:2][CH:3]=1

참가 물질

5

반응물 2

HCID 6509Tetraethylammonium HydroxideHCID 670514083-Iodophenylcarbazole

생성물 1

HCID 23509207HCID 23509207, 화합물

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 180Acetone용매

반응 조건

온도
70 °C

실험 절차

91 g (242 mmol) of 3-iodophenylcarbazole 18 and 91 g (246 mmol) of phenylcarbazoleboronic ester 19 are suspended in acetone, and a 350 ml of 20% tetraethylammonium hydroxide solution (493 mmol) are added, the mixture is carefully degassed using argon. 4.6 g (4 mmol) of tetrakistriphenylphosphinepalladium are subsequently added. The reaction is heated to 70° C. The progress of the reaction is followed by means of thin-layer chromatography. When the reaction is complete, the batch is cooled to room temperature, and the precipitated product is filtered off with suction. The crude product is recrystallised from acetonitrile, giving a beige solid.

후처리

  1. customthe mixture is carefully degassed
  2. temperaturethe batch is cooled to room temperature
  3. filtrationthe precipitated product is filtered off with suction
  4. customThe crude product is recrystallised from acetonitrile
  5. customgiving a beige solid

출처 및 근거

ORD 기록
ord-59a89d23f42d4958b1c57e05f65863fd
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969512B2

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