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Sodium Hydroxide → HCID 178526123, 화합물

HRID 2307923
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HRID 2307923 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[Cl:30])[CH2:5][N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:7]1[C:22]([O:24]CC)=[S:23].[OH-].[Na+]>C1COCC1.CO>[Cl:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[Cl:30])[CH2:5][N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:7]1[C:22]([OH:24])=[S:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 86759581HCID 86759581, 화합물

생성물 1

HCID 178526123HCID 178526123, 화합물수율 28.2%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

실험 절차

Ethyl N-(3,4-dichlorobenzyl)-3-benzylthioindole-2-carboxylate (0.31 g) was dissolved in THF/methanol (1:1) and sodium hydroxide (2M, 2.0 ml) was added and the reaction stirred for 16 hours. The reaction was then concentrated in vacuo and the residue dissolved in water. The solution was acidified by dropwise addition of acetic acid, resulting in the precipitation of a white solid which was filtered, washed with water and dried in vacuo to give the desired end product (0.082 g, 28%); NMR d (CD3SOCD3) 4.04 (s, 2H), 5.72 (s, 2H), 6.83-7.62 (m, 12H); M/z (−) 442 (M+), 440, 428, 398, 396, 307, 305.

후처리

  1. concentrationThe reaction was then concentrated in vacuo
  2. dissolutionthe residue dissolved in water
  3. additionThe solution was acidified by dropwise addition of acetic acid
  4. customresulting in the precipitation of a white solid which
  5. filtrationwas filtered
  6. washwashed with water
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-b8edb449ad2045ff8267b80c57ce8d96
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06833387B1

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