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Boron tribromide → HCID 19597475, 화합물

HRID 611525
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HRID 611525 반응식
B(Br)(Br)Br.[NH2:5][C:6]1[C:7]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([O:21]C)=[CH:17][CH:16]=3)=[CH:13][N:12]([CH:23]([CH3:25])[CH3:24])[C:8]=2[N:9]=[CH:10][N:11]=1>ClCCl>[NH2:5][C:6]1[C:7]2[C:14]([C:15]3[CH:16]=[CH:17][C:18]([OH:21])=[CH:19][CH:20]=3)=[CH:13][N:12]([CH:23]([CH3:25])[CH3:24])[C:8]=2[N:9]=[CH:10][N:11]=1
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4

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HCID 25134Boron tribromide2회HCID 195974095-(4-Methoxyphenyl)-7-(1-methylethyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine

생성물 1

HCID 19597475HCID 19597475, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

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온도
0 °C

실험 절차

A solution of boron tribromide (14.4 ml of a 1M solution in dichloromethane) was added dropwise to a stirred solution of 4-amino-7-isopropyl-5-(4-methoxyphenyl) pyrrolo[2,3-d]pyrimidine (1.35 g) in dichloromethane (100 ml) at -10° C. under nitrogen. The reaction mixture was allowed to warm to 0° C. and stirred at this temperature for one hour. Additional boron tribromide (9.6 ml of a 1M solution in dichloromethane) was added at -10° C. and the mixture was allowed to warm to 0° C. and stirred for a further hour. The reaction mixture was quenched by the dropwise addition of saturated sodium bicarbonate solution (50 ml). The mixture was allowed to stand overnight and the dichloromethane layer separated off. Insoluble material at the interface was removed by filtration and dried to yield 4-amino-5-(4-hydroxyphenyl)-7-isopropylpyrrolo-[2,3-d]pyrimidine. The structure was confirmed by 1H nmr.

후처리

  1. temperatureto warm to 0° C.
  2. stirringstirred for a further hour
  3. customThe reaction mixture was quenched by the dropwise addition of saturated sodium bicarbonate solution (50 ml)
  4. waitto stand overnight
  5. customthe dichloromethane layer separated off
  6. customInsoluble material at the interface was removed by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-c2472e42943e4e92a73cc8066a900c3a
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06001839

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