tert-Butyl isothiocyanate → N-[(2S)-2-hydroxypropyl]-N'-tert-butylthiourea

HRID 47745노트

반응식

HRID 47745 반응식
[NH2:1][CH2:2][C@@H:3]([OH:5])[CH3:4].[C:6]([N:10]=[C:11]=[S:12])([CH3:9])([CH3:8])[CH3:7]>C(O)C.C(OCC)C>[OH:5][C@@H:3]([CH3:4])[CH2:2][NH:1][C:11]([NH:10][C:6]([CH3:9])([CH3:8])[CH3:7])=[S:12]

참가 물질

5

반응물 2

HCID 11544tert-Butyl isothiocyanateHCID 7311736(S)-(+)-1-Aminopropan-2-ol

생성물 1

HCID 23381537N-[(2S)-2-hydroxypropyl]-N'-tert-butylthiourea수율 93.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

반응 조건

온도
20 °C

실험 절차

The process is performed as in Example 1, starting with 5 g of (+)-(S)-1-amino-2-propanol and 8.43 g of tert-butyl isothiocyanate in 60 cm3 of ethanol. After stirring the reaction medium for 5 hours at a temperature in the region of 20° C. and then concentration under reduced pressure (5 kPa) at a temperature in the region of 50° C., the white solid obtained is taken up in diethyl ether. The suspension is again concentrated under the same conditions as above. 11.86 g of N-[(2S)-2-hydroxypropyl]-N′-tert-butylthiourea are obtained in the form of a white solid melting at 106° C.

후처리

  1. concentrationconcentration under reduced pressure (5 kPa) at a temperature in the region of 50° C.
  2. customthe white solid obtained
  3. concentrationThe suspension is again concentrated under the same conditions as above

출처 및 근거

ORD 기록
ord-7e98585b952d43d2904d99276cac5898
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699895B2

반응 노트

불러오는 중…