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Hydrazine hydrate (1:1) → Ethyl 5-(hydrazinecarboxamido)-3-methylthiophene-2-carboxylate

HRID 560556
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인쇄 미리보기

반응식

HRID 560556 반응식
[CH3:1][C:2]1[CH:6]=[C:5]([NH:7][C:8](OC2C=CC=CC=2)=[O:9])[S:4][C:3]=1[C:17]([O:19][CH2:20][CH3:21])=[O:18].O.[NH2:23][NH2:24]>O1CCCC1>[NH:23]([C:8]([NH:7][C:5]1[S:4][C:3]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:2]([CH3:1])[CH:6]=1)=[O:9])[NH2:24]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 43403943Ethyl 3-methyl-5-(phenoxycarbonylamino)thiophene-2-carboxylate

생성물 1

HCID 66631914Ethyl 5-(hydrazinecarboxamido)-3-methylthiophene-2-carboxylate수율 89%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred suspension of ethyl 3-methyl-5-(phenoxycarbonylamino)-thiophene-2-carboxylate (18.89 g, 61.86 mmol) in tetrahydrofuran (130 mL) was added hydrazine monohydrate (19.0 mL, 391.7 mmol). The resulting reaction mixture was stirred for 2.5 h, and then concentrated in vacuo. The residue was triturated with ethyl acetate to afford ethyl 5-(hydrazinecarboxamido)-3-methylthiophene-2-carboxylate as a yellowish solid in 89% yield (13.30 g): MS (ES+) m/z 244.2 (M+1).

후처리

  1. customThe resulting reaction mixture
  2. concentrationconcentrated in vacuo
  3. customThe residue was triturated with ethyl acetate

출처 및 근거

ORD 기록
ord-b8f7234f0464487caaedf37cbaf0ee88
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063084B2

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