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Diethyl Ether → 3-(3,5-Difluorophenyl)propyl Isothiocyanate

HRID 247419
노트
인쇄 미리보기

반응식

HRID 247419 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][CH2:11][NH2:12])[CH:5]=[C:6]([F:8])[CH:7]=1.C(N(CC)CC)C.[C:20](Cl)(Cl)=[S:21].C(OCC)C>O1CCCC1>[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][CH2:11][N:12]=[C:20]=[S:21])[CH:5]=[C:6]([F:8])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 10040ThiophosgeneHCID 140499133-(3,5-Difluorophenyl)propan-1-amine

생성물 1

HCID 140499143-(3,5-Difluorophenyl)propyl Isothiocyanate수율 55%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 3-(3,5-difluorophenyl)propylamine (0.0327 mol) and triethylamine (0.072 mol) in tetrahydrofuran (20 ml) was added dropwise to a solution of thiophosgene (0.0392 mol) in tetrahydrofuran at 0°. The reaction was stirred 2 hours at room temperature then ethyl ether was added and the mixture filtered. The filtrate was concentrated and distilled (Kugelrohr) to yield 3.8 g (55%) of a yellow oil.

후처리

  1. filtrationthe mixture filtered
  2. concentrationThe filtrate was concentrated
  3. distillationdistilled (Kugelrohr)

출처 및 근거

ORD 기록
ord-b092461fe7c442fe86c3cea067b44f22
출처 데이터셋
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04707488

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