2-Chloro-1,3,5-trimethylbenzene → HCID 59531008, 화합물

HRID 1941906노트

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HRID 1941906 반응식
C1(C)C=C(C)C=C(C)C=1Cl.[OH:11][C@H:12]([C:27]1[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[CH:29][CH:28]=1)[C@H:13]([NH:16][C:17](=[O:26])[O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:14]O.[NH:35]1[CH2:39][CH2:38][CH2:37][CH2:36]1>N1C=CC=CC=1>[OH:11][C@H:12]([C:27]1[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[CH:29][CH:28]=1)[C@H:13]([NH:16][C:17](=[O:26])[O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:14][N:35]1[CH2:39][CH2:38][CH2:37][CH2:36]1

참가 물질

5

반응물 3

HCID 154622-Chloro-1,3,5-trimethylbenzeneHCID 31268PyrrolidineHCID 57331880HCID 57331880, 화합물

생성물 1

HCID 59531008HCID 59531008, 화합물수율 66%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
45 °C

실험 절차

Mesityl chloride (0.28 mL, 3.6 mmol) was added slowly to a cold (−10° C.) solution of benzyl (1R,2R)-1,3-dihydroxy-1-(4-methoxyphenyl)propan-2-ylcarbamate (1.07 g, 3.23 mmol) in pyridine (1.5 mL). The mixture was stirred for 30 min and then pyrrolidine (2.7 mL, 33 mmol) was added slowly to the mixture. The mixture was heated to 45° C. for 6 hours and then the solvent was removed to dryness. After purification by column chromatography (SiO2, using a mixture of CH2Cl2, MeOH, NH4OH), the product was obtained as a clear oil (0.816 g, 66% yield).

후처리

  1. customthe solvent was removed to dryness
  2. customAfter purification by column chromatography (SiO2
  3. additiona mixture of CH2Cl2, MeOH, NH4OH), the product

출처 및 근거

ORD 기록
ord-a6597e04e2fb4e2287a22798b8723a63
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389517B2

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