Toluene → HCID 15085579, 화합물

HRID 1607523노트

반응식

HRID 1607523 반응식
[CH3:1][O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[NH2:10])=[O:4].[CH2:11]([N:13]([CH2:16]C)CC)C.C(Cl)(Cl)=[O:19].C1(C)C=CC=CC=1>O1CCCC1>[CH3:11][NH:13][C:16](=[O:19])[NH:10][C:9]1[CH:8]=[CH:7][S:6][C:5]=1[C:3]([O:2][CH3:1])=[O:4]

참가 물질

6

반응물 4

HCID 1140TolueneHCID 6371PhosgeneHCID 8471TriethylamineHCID 89652Methyl 3-amino-2-thiophenecarboxylate

생성물 1

HCID 15085579HCID 15085579, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of methyl-3-amino-thiophene-2-carboxylate (5 g, 31,8 mmole) and triethylamine (4,43 ml, 31,8 mmole) in dry tetrahydrofuran (100 ml) was added dropwise a 20% phosgene solution in toluene (31,8 mmole). After the addition had been completed the mixture was heated to reflux for 30 min, followed by filtration at room temperature. The filtrate was evaporated in vacuo, whereafter the crystalline residue was suspended in water (200 ml). Filtration of the suspension left the title compound as white crystals. M.p. 141°-142° C.

후처리

  1. additionAfter the addition
  2. temperaturewas heated
  3. temperatureto reflux for 30 min
  4. filtrationfollowed by filtration at room temperature
  5. customThe filtrate was evaporated in vacuo, whereafter the crystalline residue
  6. filtrationFiltration of the suspension
  7. waitleft the title compound as white crystals

출처 및 근거

ORD 기록
ord-416f9324956a49c688a00cd94c5dbc9e
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04866065

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