Water → 2-(Tert-butoxycarbonylamino)acetophenone thiosemicarbazone

HRID 604591노트

반응식

HRID 604591 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[NH2:19][NH:20][C:21]([NH2:23])=[S:22].O>CO>[C:1]([O:5][C:6]([NH:8][CH2:9][C:10](=[N:19][NH:20][C:21]([NH2:23])=[S:22])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 3037943Thiosemicarbazide HydrochlorideHCID 11230079tert-butyl N-(2-oxo-2-phenylethyl)carbamate

생성물 1

HCID 866224902-(Tert-butoxycarbonylamino)acetophenone thiosemicarbazone수율 95.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2-(tert-Butoxycarbonylamino)acetophenone (3.00 g) was dissolved in methanol (21.0 mL). To the solution was added an aqueous solution (water: 9.0 mL) of thiosemicarbazide hydrochloride (3.11 g, 24.4 mmol) at room temperature. After the mixture was stirred at the same temperature for 30 minutes, water (12.0 mL) was added, and the mixture was stirred at room temperature for 20 minutes and then at 0° C. for 1 hour. The deposited solid was collected by filtration and washed with cooled 50% aqueous methanol (20 mL). The resulting solid was dried at 40° C. under reduced pressure to give seed crystals of 2-(tert-butoxycarbonylamino)acetophenone thiosemicarbazone (3.56 g, yield: 95.1%) as a white solid.

후처리

  1. stirringthe mixture was stirred at room temperature for 20 minutes
  2. waitat 0° C. for 1 hour
  3. filtrationThe deposited solid was collected by filtration
  4. washwashed
  5. temperaturewith cooled 50% aqueous methanol (20 mL)
  6. customThe resulting solid was dried at 40° C. under reduced pressure

출처 및 근거

ORD 기록
ord-0dcd86ec0dd044999c2b38e0d4a15777
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07910611B2

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