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Methyl isothiocyanate → 2'(N-methylthiocarbamyl)spiro[benzofuran-2(3H), 4'(2'H)-isoquinoline]

HRID 1758525
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반응식

HRID 1758525 반응식
[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]2([CH2:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[O:11]2)[CH2:3][NH:2]1.[CH3:19][N:20]=[C:21]=[S:22]>C1C=CC=CC=1>[CH3:19][NH:20][C:21]([N:2]1[CH2:3][C:4]2([CH2:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[O:11]2)[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH2:1]1)=[S:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11167Methyl isothiocyanateHCID 15917444spiro[benzofuran-2(3H),4'(2'H)-isoquinoline]

생성물 1

HCID 132645342'(N-methylthiocarbamyl)spiro[benzofuran-2(3H), 4'(2'H)-isoquinoline]

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

To a stirred solution of spiro[benzofuran-2(3H),4'(2'H)-isoquinoline] (5.0 g) in dry benzene (18 ml) is added methylisothiocyanate (3.1 g) in dry benzene (10 ml). After one hour, the product begins to separate. The mixture is stirred overnight and diluted with hexane (18 ml). The product is filtered, washed with hexane and dried to yield a solid. The solid is twice recrystallized from benzene to yield (3.0 g, 46%) as a solid, mp 165°.166°.

후처리

  1. customto separate
  2. additiondiluted with hexane (18 ml)
  3. filtrationThe product is filtered
  4. washwashed with hexane
  5. customdried
  6. customto yield a solid
  7. customThe solid is twice recrystallized from benzene
  8. customto yield (3.0 g, 46%) as a solid, mp 165°
  9. custom166°

출처 및 근거

ORD 기록
ord-b65e2fc82fe84c20bced951817e0ed73
출처 데이터셋
uspto-grants-1983_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04374137

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