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Lithium Hydroxide → N-[1-ethyl-1-(hydroxymethyl)propyl]thiourea

HRID 1992559
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HRID 1992559 반응식
[CH2:1]([C:3]([NH:8][C:9]([NH:11]C(=O)C1C=CC=CC=1)=[S:10])([CH2:6][OH:7])[CH2:4][CH3:5])[CH3:2].[Li+].[OH-]>O1CCCC1.CO.O>[CH2:1]([C:3]([NH:8][C:9]([NH2:11])=[S:10])([CH2:6][OH:7])[CH2:4][CH3:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 3939Lithium HydroxideHCID 86618579N-({[1-ethyl-1-(hydroxymethyl)propyl]amino}carbonothioyl)benzamide

생성물 1

HCID 86618580N-[1-ethyl-1-(hydroxymethyl)propyl]thiourea수율 68%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran
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실험 절차

A solution of N-({[1-ethyl-1-(hydroxymethyl)propyl]amino}carbonothioyl)benzamide (6.8779 g, 24.5 mmol), prepared in the previous step, and 1 M LiOH (29.4 mL, 29.4 mmol) in 200 mL of tetrahydrofuran plus 200 mL of methanol plus 100 mL of water was stirred under nitrogen at room temperature for 21 h. The reaction was concentrated under reduced pressure to remove most of the tetrahydrofuran and methanol. The solid present was collected by filtration and dried under reduced pressure to give N-[1-ethyl-1-(hydroxymethyl)propyl]thiourea (2.9228 g, 68%) as a white solid, mp 148-151° C.; MS (ESI) m/z 177 [M+H]+.

후처리

  1. concentrationThe reaction was concentrated under reduced pressure
  2. customto remove most of the tetrahydrofuran and methanol
  3. filtrationThe solid present was collected by filtration
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-8f64ac30f4764b508a625111bcff1c49
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07649007B2

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