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Sodium Acetate → 2-Amino-5-methyl-4,5,6-trihydrobenzothiazol-7-one

HRID 1468696
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HRID 1468696 반응식
Br[CH:2]1[C:7](=[O:8])[CH2:6][CH:5]([CH3:9])[CH2:4][C:3]1=O.C([O-])(=O)C.[Na+].[NH2:16][C:17]([NH2:19])=[S:18]>C(O)(=O)C>[NH2:19][C:17]1[S:18][C:2]2[C:7](=[O:8])[CH2:6][CH:5]([CH3:9])[CH2:4][C:3]=2[N:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 2723790ThioureaHCID 669327192-Bromo-5-methylcyclohexane-1,3-dione

생성물 1

HCID 27565102-Amino-5-methyl-4,5,6-trihydrobenzothiazol-7-one

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

To a solution of 24 in acetic acid (540 mL) was added sodium acetate (44.3 g, 540 mmol) and thiourea (28.8 g, 378 mmol). The reaction mixture was stirred with a mechanical stirrer at 100° C. for 3 h. The reaction mixture was partially concentrated in vacuo. EtOAc was added (500 mL). The mixture was made basic with 1 M NaOH, and the layers were separated. The aqueous layer was extracted with EtOAc (2×300 mL). The combined organic layers were dried, filtered, and concentrated in vacuo to give 49.3 g of 25, which was taken on without further purification.

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후처리

  1. concentrationThe reaction mixture was partially concentrated in vacuo
  2. additionEtOAc was added (500 mL)
  3. customthe layers were separated
  4. extractionThe aqueous layer was extracted with EtOAc (2×300 mL)
  5. customThe combined organic layers were dried
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5a35312db4704ff4bf19d9e36ce8f81b
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006229B2

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